Category: 70261-81-3

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.70261-81-3,1-Methyl-4-(4-nitrobenzyl)piperazine,as a common compound, the synthetic route is as follows.

70261-81-3, EXAMPLE 3 4-((4-methyl-1-piperazinyl)methyl)aniline (I-c) Crude I-a (8.5g, 36.2mmol), FeO(OH)/C, 2.0 g as catalyst and 95% ethanol (100 ml) were added into a 500 mL single neck flask, which was refluxed. Into the reaction system were added slowly and dropwise a mixture of 25 mL hydrazine hydrate and 20 mL 95% ethanol. The depletion of the starting materials was confirmed by TLC (methanol: chloroform = 1:15). Suction filtration was performed while the reaction mixture was hot. The filter cake was washed with hot ethanol twice (30 ml *2). After removal of the solvent under reduced pressure, white solid was obtained, which was dried under vacuum to give 6.7 g (I-c); Yield: 90.3%. The product was used for subsequent reaction without further purification. 1H-NMR[300MHz, DMSO-d6]: delta2.1 (3H, s, -CH3), 2.3-2.5 (8H, m, -CH2-*4), 3.5 (2H, s, -CH2-), 4.0(2H, s, -NH2), 7.5 (2H, d, J = 8.7 Hz, ArH), 8.1 (2H, d, J = 8.7 Hz, ArH).

As the paragraph descriping shows that 70261-81-3 is playing an increasingly important role.

Reference：
Patent; China Pharmaceutical University; LU, Tao; WANG, Yue; CHEN, Yadong; LU, Yi; WANG, Zhanwei; JIN, Qiaomei; YANG, Taotao; LIN, Guowu; GUO, Qinglong; ZHAO, Li; EP2955185; (2015); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.70261-81-3,1-Methyl-4-(4-nitrobenzyl)piperazine,as a common compound, the synthetic route is as follows.

70261-81-3, EXAMPLE 3 4-((4-methyl-1-piperazinyl)methyl)aniline (I-c) Crude I-a (8.5g, 36.2mmol), FeO(OH)/C, 2.0 g as catalyst and 95% ethanol (100 ml) were added into a 500 mL single neck flask, which was refluxed. Into the reaction system were added slowly and dropwise a mixture of 25 mL hydrazine hydrate and 20 mL 95% ethanol. The depletion of the starting materials was confirmed by TLC (methanol: chloroform = 1:15). Suction filtration was performed while the reaction mixture was hot. The filter cake was washed with hot ethanol twice (30 ml *2). After removal of the solvent under reduced pressure, white solid was obtained, which was dried under vacuum to give 6.7 g (I-c); Yield: 90.3%. The product was used for subsequent reaction without further purification. 1H-NMR[300MHz, DMSO-d6]: delta2.1 (3H, s, -CH3), 2.3-2.5 (8H, m, -CH2-*4), 3.5 (2H, s, -CH2-), 4.0(2H, s, -NH2), 7.5 (2H, d, J = 8.7 Hz, ArH), 8.1 (2H, d, J = 8.7 Hz, ArH).

As the paragraph descriping shows that 70261-81-3 is playing an increasingly important role.

Reference：
Patent; China Pharmaceutical University; LU, Tao; WANG, Yue; CHEN, Yadong; LU, Yi; WANG, Zhanwei; JIN, Qiaomei; YANG, Taotao; LIN, Guowu; GUO, Qinglong; ZHAO, Li; EP2955185; (2015); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.70261-81-3,1-Methyl-4-(4-nitrobenzyl)piperazine,as a common compound, the synthetic route is as follows.

General Procedure 3-1 : Synthesis of (4-((4-methylpiperazin-l-yl)methyl)aniline)[00187] The synthesis of the title compound was conducted as described in U.S. Pat. Appl. Publ.No. 2006058341 (March 16, 2006). Specifically, to a solution of 4-nitrobenzyl chloride in THF at the room temperature was added 1 -methyl piperazine. The solution was stirred for 3 hours after which time the crude reaction was diluted with ethyl acetate and washed repeatedly with water. The dried organics were concentrated to give directly the 4-nitrobenzylamine adduct.This was subsequently treated with Rainey Nickel in THF at 75PSI for 12 hours to give the title compound., 70261-81-3

70261-81-3 1-Methyl-4-(4-nitrobenzyl)piperazine 677795, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; BIOGEN IDEC MA INC.; WO2008/94575; (2008); A2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

70261-81-3, 1-Methyl-4-(4-nitrobenzyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

70261-81-3, 4-Amino-N-[4-[(4-methylpiperazin-1-yl) methyl] phenyl]-1Hpyrazole-3-carboxamide (5): The mixture of N-methylpiperazine (4.9 mL, 44.2 mmol) and triethylamine (12 mL,86.3 mmol) in dichloromethane (20 mL) was added dropwiseto a stirred solution of Nitro-benzyl bromide 1 (10.0 mg,46.3 mmol) in dichloromethane (100 mL) under the ice-waterbath and was refluxed for 1 h. The reaction mixture was extractedwith chloroform (100 mL×3), washed with water andsaturated sodium chloride each time (100 mL×1). The organicphase was dried with anhydrous magnesium sulfate, filtered,evaporated under vacuum to give pale yellow solid 2. Withoutfurther purification, 2 mixed with FeO(OH)/C (catalyst 2.0 g)and 95% ethanol (100 mL) were kept refluxing and dropwiseadded the mixture of hydrazine hydrate (25 mL) and 95%ethanol (20 mL), then filtrated when the solution was hot. Theresidue was washed with hot ethanol (30 mL×2). The solventwas distilled under vacuum to give white solid 3 (6.7 g), thenmixed with 4-nitro-1H-pyrazole-3-acid (6.3 g, 40.0 mmol),EDCI (8.4 g, 43.8 mmol) and HOBT (6.0 g, 44.4 mmol) in anhydrousDMF (100 mL), stirred for 24 h at room temperature.The reaction mixture was poured into ice water (200 mL).A large amount of yellow solid precipitation was acquired.The pure product 4 was got from recrystallizing with mixedsolvent of methanol and ethyl acetate, then the same processof hydrazine hydrate reduction was done with the catalyst ofFeO(OH)/C. The solvent was distilled under vacuum to give white solid 5 (3.5 g). Yield= 63.9%; mp 199-201C; IR (KBr)cm-1: 3369, 3227 (NH2), 1346 (C= C), 1456 (C= N) pyrazole,646 (ArH); 1H-NMR (300 MHz, DMSO-d6) delta (ppm): 2.1 (3H,s, -CH3), 2.3-2.5 (8H, m, -CH2-), 3.3 (2H, s, -CH2-), 4.7(1H, s, -NH2), 7.1-7.2 (3H, m, ArH), 7.7 (2H, d, J=10.5 Hz,ArH), 9.7 (1H, s, -NHCO-), 12.7 (1H, s, Pyrazole); MS m/z:315.82 (M+); Anal. Calcd for C16H22N6O: C, 61.13; H, 7.05; N,26.73; O, 5.09. Found: C, 61.31; H, 6.84; N, 26.52.

70261-81-3 1-Methyl-4-(4-nitrobenzyl)piperazine 677795, apiperazines compound, is more and more widely used in various fields.

Reference：
Article; Lu, Yi; Ran, Ting; Lin, Guowu; Jin, Qiaomei; Jin, Jianling; Li, Hongmei; Guo, Hao; Lu, Tao; Wang, Yue; Chemical and Pharmaceutical Bulletin; vol. 62; 3; (2014); p. 238 – 246;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

70261-81-3, 1-Methyl-4-(4-nitrobenzyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

70261-81-3, 4-Amino-N-[4-[(4-methylpiperazin-1-yl) methyl] phenyl]-1Hpyrazole-3-carboxamide (5): The mixture of N-methylpiperazine (4.9 mL, 44.2 mmol) and triethylamine (12 mL,86.3 mmol) in dichloromethane (20 mL) was added dropwiseto a stirred solution of Nitro-benzyl bromide 1 (10.0 mg,46.3 mmol) in dichloromethane (100 mL) under the ice-waterbath and was refluxed for 1 h. The reaction mixture was extractedwith chloroform (100 mL×3), washed with water andsaturated sodium chloride each time (100 mL×1). The organicphase was dried with anhydrous magnesium sulfate, filtered,evaporated under vacuum to give pale yellow solid 2. Withoutfurther purification, 2 mixed with FeO(OH)/C (catalyst 2.0 g)and 95% ethanol (100 mL) were kept refluxing and dropwiseadded the mixture of hydrazine hydrate (25 mL) and 95%ethanol (20 mL), then filtrated when the solution was hot. Theresidue was washed with hot ethanol (30 mL×2). The solventwas distilled under vacuum to give white solid 3 (6.7 g), thenmixed with 4-nitro-1H-pyrazole-3-acid (6.3 g, 40.0 mmol),EDCI (8.4 g, 43.8 mmol) and HOBT (6.0 g, 44.4 mmol) in anhydrousDMF (100 mL), stirred for 24 h at room temperature.The reaction mixture was poured into ice water (200 mL).A large amount of yellow solid precipitation was acquired.The pure product 4 was got from recrystallizing with mixedsolvent of methanol and ethyl acetate, then the same processof hydrazine hydrate reduction was done with the catalyst ofFeO(OH)/C. The solvent was distilled under vacuum to give white solid 5 (3.5 g). Yield= 63.9%; mp 199-201C; IR (KBr)cm-1: 3369, 3227 (NH2), 1346 (C= C), 1456 (C= N) pyrazole,646 (ArH); 1H-NMR (300 MHz, DMSO-d6) delta (ppm): 2.1 (3H,s, -CH3), 2.3-2.5 (8H, m, -CH2-), 3.3 (2H, s, -CH2-), 4.7(1H, s, -NH2), 7.1-7.2 (3H, m, ArH), 7.7 (2H, d, J=10.5 Hz,ArH), 9.7 (1H, s, -NHCO-), 12.7 (1H, s, Pyrazole); MS m/z:315.82 (M+); Anal. Calcd for C16H22N6O: C, 61.13; H, 7.05; N,26.73; O, 5.09. Found: C, 61.31; H, 6.84; N, 26.52.

70261-81-3 1-Methyl-4-(4-nitrobenzyl)piperazine 677795, apiperazines compound, is more and more widely used in various fields.

Reference：
Article; Lu, Yi; Ran, Ting; Lin, Guowu; Jin, Qiaomei; Jin, Jianling; Li, Hongmei; Guo, Hao; Lu, Tao; Wang, Yue; Chemical and Pharmaceutical Bulletin; vol. 62; 3; (2014); p. 238 – 246;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.70261-81-3,1-Methyl-4-(4-nitrobenzyl)piperazine,as a common compound, the synthetic route is as follows.

70261-81-3, To a 0 0C cooled solution of 4-nitrobenzaldehyde in DCM (40 mL) was added Na(OAc)3BH (10.526gm, 49.66 mmol) and the reacton was stirred for lOmin. To the reaction mixture was added N-methylpiperazine (9.93 g, 99.3 mmol) under nitrogen atmosphere and the reaction mixture was continued stirring at room temperature for 4h. The progress of the reaction was monitored by TLC and upon completion of the reaction, the mixture was partitioned between DCM (20 mL) and water (15 mL) and the organic layer was separated, washed with water (2 x 15 mL), dried over sodium sulphate, filtered and the solvent was removed under reduced pressure to give crude residue. Washing with ether gave l-methyl-4-(4-nitrobenzyl)piperazine (4 g). 1H NMR (CDCl3, 200MHz) delta: 8.19 (2H, d, J= 8.4Hz), 7.53 (2H5 d, J= 8.4 Hz)5 3.59 (2H, s), 2.47 (8H, bm), 2.29 (3H5 s); m/e = 236 (M+l). To a solution of l-methyl-4-(4-nitrobenzyl)piperazine (4.0 g) in methanol (100 niL) at room temperature under nitrogen atmosphere was added Raney nickel (1.6gm). The reaction mixture was stirred for 2 hr under hydrogen atmosphere. The progress of the reaction was monitored by TLC and upon completion of the reaction, the mixture was filtered under nitrogen atmosphere and the solvent was removed under reduced pressure to give 4-[(4-methylpiperazin-l-yl)methyl]aniline (3.2 g). 1H NMR (CDCl3, 200MHz) delta: 7.13 (2H, d, J= 8.4 Hz)5 6.61 (2H, d5 J= 8.4 Hz), 3.41 (2H, s), 2.45 (8H, bm), 2.27 (3H, s); m/e = 206 (M+l).To a stirred solution of 4-[(4-methylpiperazin-l-yl)methyl]aniline (3.2 g, 15.57 mmol) in acetic acid: concentrated HCl (32:32 niL) at 10 0C was added NaNO2 (1.30 g,18.78 mmol) in water (16 mL) and stirred for 10 min. Freshly prepared SnCl2^H2O (11.75 g, 51.97 mmol) in concentrated HCl (32 mL) was added at 10 0C. The temperature of the reaction mixture was allowed to rise to room temperature and maintained there for 4hr. After filtering the reaction mixture, the precipitate was washed with water and the solid obtained was dried under reduced pressure to obtain l-(4-hydrazmobenzyl)-4- methylpiperazine (3.4 g). 1HNMR (CD3OD, 200MHz) delta: 7.66 (2H, d, J= 8.4 Hz), 7.13 (2H, d, J= 8.4 Hz), 4.46 (2H, s), 3.72 (8H5 bm), 3.11 (3H5 s);To a solution of l-(4-hydrazinobenzyl)-4-methylpiperazine (3.4 g, 13.25 mmol) in ethanol (50 mL) were added piperidone. HCl (2.51 g, 18.55 mmol). The reaction temperature was raised to 90 0C and continued stirring for 2 hrs. The progress of the reaction was monitored by TLC and upon completion of the reaction the mixture was cooled to rt and HCl gas was bubbled through the reaction mixture at 0 0C. After the reaction mixture was saturated with HCl, the temperature was raised to 90 0C again and continued stirring for 2hrs. The ethanolic HCl was removed under reduced pressure and the pH of the reaction mixture was adjusted to 12.0 with 10% NaOH solution. The mixture was partitioned between 20% MeOH: DCM and water (35 mL) and the organic layer was separated, dried over Na2SO4 filtered and the solvent was removed under reduced pressure to give crude residue. Washing with ether gave 8-[(4-methylpiperazin-l-yl)methyl]-2,3,4,5- tetrahydro-lNo.-pyrido[4,3-&]indole (1 g). 1HNMR(CD3OD5 200MHz) delta: 7.31 (IH, s), 7.27 (IH, d, J= 8.6 Hz), 7.06 (IH, d, J= 8.6 Hz), 4.01 (2H5 s), 3.60 (2H, s), 3.21 (8H5 bm), 2.86 (4H5 m), 2.28 (3H, s); m/e = 285 (M+l).To a solution of 8-[(4-methylpiperazin-l-yl)methyl]-2,3,4,5-tetrahydro-li- pyrido[4,3-delta]indole(0.5 g,1.76 mmol) in DMF (15 mL) at rt was added Example 7 (0.567 g, 2.64 mmol) and K2CO3 (0.731 g, 5.28 mmol). The reaction temperature was raised to 100 0C and continued stirring for 12hr. The progress of the reaction was monitored by TLC and upon completion of the reaction DMF was removed under reduced pressure. The reaction mixture was partitioned between ethyl acetate (100 mL) and water (80 mL) and the organic layer was separated, dried over sodium sulphate, filtered and the solvent was removed under reduced pressure to give crude residue. Washing with ether gave methyl 2-{8-[(4- methylpiperazin-1 -yl)methyl]-l 53s4,5-tetrahydro-2H-pyrido[4,3-b]indol-2-yl}pyrimidine-5- carboxylate (0.15 g). 1HNMR (DMSO-D6, 200MHz) delta: 8.84 (2H, s), 7.94 (lH,s), 7.67 (IH, d, J= 8.6 Hz), 7.54 (IH, d, J= 8.6 Hz), 5.01 (2H, s), 3.80-3.01 (1OH, m), 2.87 (3H, s); m/e = 421 (M+l).To a 00C solution of methyl 2-{8-[(4-methylpiperazin~l-yl)methyl]-l,3,4,5- tetrahydro-2H-pyrido[4,3-b]indol-2-yl}pyrimidine-5-carboxylate (0.1 g) in MeOH: DCM (5:2 mL) was added 50% aqueous hydroxylamine solution (2 mL) and to the mixture was added a solution of NaOH (0.08 g) in water (1 mL). The reaction mixture was stirred at room temperature for lhr and the progress of the reaction was monitored by TLC and upon completion of the reaction the solvent was removed under reduced pressure. The pH of the mixture was adjusted to 7.5 using IN HCl and the obtained solid was filtered and washed with water followed by diethyl ether. After filtering, t…

70261-81-3 1-Methyl-4-(4-nitrobenzyl)piperazine 677795, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; MIKANA THERAPEUTICS, INC.; WO2006/88949; (2006); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.70261-81-3,1-Methyl-4-(4-nitrobenzyl)piperazine,as a common compound, the synthetic route is as follows.

70261-81-3, To a 0 0C cooled solution of 4-nitrobenzaldehyde in DCM (40 mL) was added Na(OAc)3BH (10.526gm, 49.66 mmol) and the reacton was stirred for lOmin. To the reaction mixture was added N-methylpiperazine (9.93 g, 99.3 mmol) under nitrogen atmosphere and the reaction mixture was continued stirring at room temperature for 4h. The progress of the reaction was monitored by TLC and upon completion of the reaction, the mixture was partitioned between DCM (20 mL) and water (15 mL) and the organic layer was separated, washed with water (2 x 15 mL), dried over sodium sulphate, filtered and the solvent was removed under reduced pressure to give crude residue. Washing with ether gave l-methyl-4-(4-nitrobenzyl)piperazine (4 g). 1H NMR (CDCl3, 200MHz) delta: 8.19 (2H, d, J= 8.4Hz), 7.53 (2H5 d, J= 8.4 Hz)5 3.59 (2H, s), 2.47 (8H, bm), 2.29 (3H5 s); m/e = 236 (M+l). To a solution of l-methyl-4-(4-nitrobenzyl)piperazine (4.0 g) in methanol (100 niL) at room temperature under nitrogen atmosphere was added Raney nickel (1.6gm). The reaction mixture was stirred for 2 hr under hydrogen atmosphere. The progress of the reaction was monitored by TLC and upon completion of the reaction, the mixture was filtered under nitrogen atmosphere and the solvent was removed under reduced pressure to give 4-[(4-methylpiperazin-l-yl)methyl]aniline (3.2 g). 1H NMR (CDCl3, 200MHz) delta: 7.13 (2H, d, J= 8.4 Hz)5 6.61 (2H, d5 J= 8.4 Hz), 3.41 (2H, s), 2.45 (8H, bm), 2.27 (3H, s); m/e = 206 (M+l).To a stirred solution of 4-[(4-methylpiperazin-l-yl)methyl]aniline (3.2 g, 15.57 mmol) in acetic acid: concentrated HCl (32:32 niL) at 10 0C was added NaNO2 (1.30 g,18.78 mmol) in water (16 mL) and stirred for 10 min. Freshly prepared SnCl2^H2O (11.75 g, 51.97 mmol) in concentrated HCl (32 mL) was added at 10 0C. The temperature of the reaction mixture was allowed to rise to room temperature and maintained there for 4hr. After filtering the reaction mixture, the precipitate was washed with water and the solid obtained was dried under reduced pressure to obtain l-(4-hydrazmobenzyl)-4- methylpiperazine (3.4 g). 1HNMR (CD3OD, 200MHz) delta: 7.66 (2H, d, J= 8.4 Hz), 7.13 (2H, d, J= 8.4 Hz), 4.46 (2H, s), 3.72 (8H5 bm), 3.11 (3H5 s);To a solution of l-(4-hydrazinobenzyl)-4-methylpiperazine (3.4 g, 13.25 mmol) in ethanol (50 mL) were added piperidone. HCl (2.51 g, 18.55 mmol). The reaction temperature was raised to 90 0C and continued stirring for 2 hrs. The progress of the reaction was monitored by TLC and upon completion of the reaction the mixture was cooled to rt and HCl gas was bubbled through the reaction mixture at 0 0C. After the reaction mixture was saturated with HCl, the temperature was raised to 90 0C again and continued stirring for 2hrs. The ethanolic HCl was removed under reduced pressure and the pH of the reaction mixture was adjusted to 12.0 with 10% NaOH solution. The mixture was partitioned between 20% MeOH: DCM and water (35 mL) and the organic layer was separated, dried over Na2SO4 filtered and the solvent was removed under reduced pressure to give crude residue. Washing with ether gave 8-[(4-methylpiperazin-l-yl)methyl]-2,3,4,5- tetrahydro-lNo.-pyrido[4,3-&]indole (1 g). 1HNMR(CD3OD5 200MHz) delta: 7.31 (IH, s), 7.27 (IH, d, J= 8.6 Hz), 7.06 (IH, d, J= 8.6 Hz), 4.01 (2H5 s), 3.60 (2H, s), 3.21 (8H5 bm), 2.86 (4H5 m), 2.28 (3H, s); m/e = 285 (M+l).To a solution of 8-[(4-methylpiperazin-l-yl)methyl]-2,3,4,5-tetrahydro-li- pyrido[4,3-delta]indole(0.5 g,1.76 mmol) in DMF (15 mL) at rt was added Example 7 (0.567 g, 2.64 mmol) and K2CO3 (0.731 g, 5.28 mmol). The reaction temperature was raised to 100 0C and continued stirring for 12hr. The progress of the reaction was monitored by TLC and upon completion of the reaction DMF was removed under reduced pressure. The reaction mixture was partitioned between ethyl acetate (100 mL) and water (80 mL) and the organic layer was separated, dried over sodium sulphate, filtered and the solvent was removed under reduced pressure to give crude residue. Washing with ether gave methyl 2-{8-[(4- methylpiperazin-1 -yl)methyl]-l 53s4,5-tetrahydro-2H-pyrido[4,3-b]indol-2-yl}pyrimidine-5- carboxylate (0.15 g). 1HNMR (DMSO-D6, 200MHz) delta: 8.84 (2H, s), 7.94 (lH,s), 7.67 (IH, d, J= 8.6 Hz), 7.54 (IH, d, J= 8.6 Hz), 5.01 (2H, s), 3.80-3.01 (1OH, m), 2.87 (3H, s); m/e = 421 (M+l).To a 00C solution of methyl 2-{8-[(4-methylpiperazin~l-yl)methyl]-l,3,4,5- tetrahydro-2H-pyrido[4,3-b]indol-2-yl}pyrimidine-5-carboxylate (0.1 g) in MeOH: DCM (5:2 mL) was added 50% aqueous hydroxylamine solution (2 mL) and to the mixture was added a solution of NaOH (0.08 g) in water (1 mL). The reaction mixture was stirred at room temperature for lhr and the progress of the reaction was monitored by TLC and upon completion of the reaction the solvent was removed under reduced pressure. The pH of the mixture was adjusted to 7.5 using IN HCl and the obtained solid was filtered and washed with water followed by diethyl ether. After filtering, t…

70261-81-3 1-Methyl-4-(4-nitrobenzyl)piperazine 677795, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; MIKANA THERAPEUTICS, INC.; WO2006/88949; (2006); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

70261-81-3,70261-81-3, 1-Methyl-4-(4-nitrobenzyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

The Second Step: Preparation of 4-(4-methylpiperazin-1-ylmethyl)phenylamine (F652-02) 1-methyl-4-(4-nitrobenzyl)-piperazine (F652-01, 4.67 g, 19.9 mmol), methanol (100 mL), zinc powder (6.5 g, 99.3 mmol) and ammonium chloride (4.3 g, 79.5 mmol) were placed in a reaction vessel and heated for 2 hours under reflux. After returning to room temperature, the reaction mixture was filtered through Celite. The solvent of the filtrate was distilled off under reduced pressure to obtain a solid. Diethyl ether was added to the solid, and insoluble components were removed by filtration. 4-(4-methylpiperazin-1-ylmethyl)phenylamine (F652-02, white solid, 3.16 g, 77%) was obtained by removing the solvent of the filtrate by distillation. LC/MS (Method 6): m/z(ESI, POS): 206[M+H]+; retention time: 1.15 minutes. 1H-NMR(400MHz, DMSO-d6)delta 2.12(s, 3H), 2.29(bs, 8H), 3.23(s, 2H), 4.93(s, 2H), 6.49(d, J=8.4Hz, 2H), 6.89(d, J=8.4Hz, 2H).

The synthetic route of 70261-81-3 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; NIPPON KAYAKU KABUSHIKI KAISHA; EP1857446; (2007); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

70261-81-3, 1-Methyl-4-(4-nitrobenzyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

70261-81-3, To the 500 mL single neck flask was added 8.5 g (36.2 mmol) of crude I-a,FeO (OH) / C catalyst 2.0 g and 95% ethanol 100 mL,Heating reflux,A mixture of 25 mL of hydrazine hydrate and 20 mL of 95% ethanol was slowly added dropwise,TLC detects the disappearance of the starting material (methanol: chloroform = 1:15).The filter cake was washed twice with hot ethanol (30 mL x 2)The solvent was evaporated under reduced pressure to give a white solid,And dried in vacuo to give 6.7 g of (I-b) in a yield of 90.3%.Products without further purification, directly into the next step.

The synthetic route of 70261-81-3 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; China Pharmaceutical University; Lu Shuai; Wang Yue; Zhi Yanle; Yao Chao; Lu Tao; Li Baoquan; Chen Puzhou; Bao Jiyin; (27 pag.)CN107245073; (2017); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.70261-81-3,1-Methyl-4-(4-nitrobenzyl)piperazine,as a common compound, the synthetic route is as follows.

Add 8.5 g (36.2 mmol) of crude I-a to a 500 mL one-necked flask. 2.0 g of FeO(OH)/C catalyst and 100 mL of 95% ethanol, Heating back, Slowly add a mixture of 25 mL of hydrazine hydrate and 20 mL of 95% ethanol. The disappearance of the starting material by TLC (methanol: chloroform = 1:15). Hot and suction filtration, The filter cake was washed twice with hot ethanol (30 mL x 2). The solvent was evaporated under reduced pressure to give a white solid. It was dried under vacuum to give (I-b) 6.7 g, yield: 90.3%. The product was directly fed to the next reaction without further purification.

70261-81-3, As the paragraph descriping shows that 70261-81-3 is playing an increasingly important role.

Reference：
Patent; China Pharmaceutical University; Wang Yue; Lu Shuai; Zhi Yanle; Yao Chao; Lu Tao; Li Baoquan; Chen Puzhou; Bao Jiyin; (26 pag.)CN109970717; (2019); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics