Category: 934-98-5

934-98-5, 2-(4-Methylpiperazin-1-yl)ethanamine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Preparation of Lambda^2-benzyl-6-(6,7-dimethoxy-3,4-dihydroisoquinolin-2(lH)-yl)-Lambda^-(2- (4-methylpiperazin-l-yl)ethyl)-l,3,5-triazine-2,4-diamineTo the above reaction solution of N-benzyl-4-chloro-6-(6,7-dimethoxy-3,4- dihydroisoquinolin-2(lH)-yl)-l,3,5-triazin-2-amine (0.126 mmol, 1 equivalent) in CEta3CNu/Eta2O (1/1, 2 ml) was added 2-(4-methyl-piperazin-l-yl)-ethylamine (36 mg, 0.252 mmol, 2 equivalents), followed by adding IN NaOH (126 mul, 0.126 mmol, 1 equivalent). The reaction mixture was heated at 8O0C overnight. The solvent was evaporated and the residue was acidified and purified with RP-HPLC (Luna, 5mu C8(2), 100x21mm, 10-60percent CH3CN/H2O, 0.1percent TFA, 17 min) to give the desired product. MS: cacld for C28H38N8O2+H+ 519.32, found 519.4., 934-98-5

As the paragraph descriping shows that 934-98-5 is playing an increasingly important role.

Reference：
Patent; PRAECIS PHARMACEUTICALS INC; DING, Yun; WO2010/85246; (2010); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

934-98-5,With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.934-98-5,2-(4-Methylpiperazin-1-yl)ethanamine,as a common compound, the synthetic route is as follows.

A solution of 2,4-dichloro-5,7-difluoro-3-nitroquinoline (5.58 gm, 2.0×10?2 moles) in 2-methyl tetrahydrofuran (50 mL) is stirred as diisopropylethylamine (2.84 gm, 2.2×10?2 moles) and N-2-aminoethyl-N? methylpiperazine (3.15 gm, 2.2×10?2 moles) are added. This solution is stirred at room temperature overnight. The yellow reaction mixture is diluted with more 2-methyl-tetrahydrofuran (50 mL) and this is washed with water (100 mL) followed by brine (50 mL). After being dried over magnesium sulfate, the solution is filtered and the solvent is removed under reduced pressure. The oily residue is stirred with diethyl ether (25 mL) and this is cooled on ice causing the product to crystallize. The solid yellow product is isolated by filtration, washed with ether and dried. The yield is about 4.32 gm.

The synthetic route of 934-98-5 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; JANUS BIOTHERAPEUTICS, INC.; Lipford, Grayson B.; Zepp, Charles M.; (72 pag.)US9873694; (2018); B2;,
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.934-98-5,2-(4-Methylpiperazin-1-yl)ethanamine,as a common compound, the synthetic route is as follows.,934-98-5

Example 53: -r2-(4-methv.-piDerazin-1 -vn-ethvi1-3-r3-(5-thioDhen-3-vi-Dvrimidin-2-viamino)-Dhenvt1-urea; To a stirring solution of W (100 mg, 0.23 mmol) in CH2CI2 (20 mL) was added J (33 mg, 0.23 mmol) followed by triethylamine (32 muL, 0.23 mmol). The solution was stirred at room temperature for 12 hours where the reaction was diluted with CH2Cl2 (50 mL) and washed with 2N NaOH (2 x 50 mL), water (2 x 50 mL) and brine (2 x 50 mL). The organics were dried over Na2S04 and concentrated in vacuo. The residue was purified using column chromatography (silica gel, 5percent MeOH in CH2CI2). The fractions containing product were evaporated to dryness under vacuum to yield compound 53 in 45percent yield as a white solid. (at)H NMR (300 MHz, CD30D) No. 2.27 (s, 3H), 2.33-2.55 (m, 7.01-7.02 (m, 1H), 7.04-7.05 (m, 2H), 7.43 (d, 1 H), 7.45 (d, 1 H), 7.64 (d, 1 H), 7.86 (d, 1 H), 8.72 (s, 2H). MS m/z 438 [M++1].

As the paragraph descriping shows that 934-98-5 is playing an increasingly important role.

Reference：
Patent; SUGEN, INC.; WO2005/113548; (2005); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

934-98-5, 2-(4-Methylpiperazin-1-yl)ethanamine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

934-98-5, General procedure: General procedure: Hydroxylamine hydrochloride (1.58 mmol)and sodium hydroxide (2.65 mmol) were added to an ice-cooledsuspension of the proper ketone compound (0.53 mmol) in 10 mlof a mixture of ethanol/H2O (2:1). After stirring for 15 min at rt,the mixture was refluxed for 2 h. The ethanol was evaporatedand the alkaline aqueous solution was neutralized with 1N HCl.When possible, the obtained suspension was filtered and the aqueoussolution was extracted with CH2Cl2 and the organic layer wasdried with anhydrous Na2SO4 and evaporated to dryness. Thecrude residue was purified as indicated for each compound.

The synthetic route of 934-98-5 has been constantly updated, and we look forward to future research findings.

Reference：
Article; Barteselli, Anna; Parapini, Silvia; Basilico, Nicoletta; Mommo, Danilo; Sparatore, Anna; Bioorganic and Medicinal Chemistry; vol. 22; 21; (2014); p. 5757 – 5765;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

934-98-5, 2-(4-Methylpiperazin-1-yl)ethanamine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

934-98-5, General procedure: General procedure: Hydroxylamine hydrochloride (1.58 mmol)and sodium hydroxide (2.65 mmol) were added to an ice-cooledsuspension of the proper ketone compound (0.53 mmol) in 10 mlof a mixture of ethanol/H2O (2:1). After stirring for 15 min at rt,the mixture was refluxed for 2 h. The ethanol was evaporatedand the alkaline aqueous solution was neutralized with 1N HCl.When possible, the obtained suspension was filtered and the aqueoussolution was extracted with CH2Cl2 and the organic layer wasdried with anhydrous Na2SO4 and evaporated to dryness. Thecrude residue was purified as indicated for each compound.

The synthetic route of 934-98-5 has been constantly updated, and we look forward to future research findings.

Reference：
Article; Barteselli, Anna; Parapini, Silvia; Basilico, Nicoletta; Mommo, Danilo; Sparatore, Anna; Bioorganic and Medicinal Chemistry; vol. 22; 21; (2014); p. 5757 – 5765;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

934-98-5, 2-(4-Methylpiperazin-1-yl)ethanamine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A 250 mL round bottom flask equipped with a stir bar was charged with Example 1U (1.96 g) and anhydrous dichloromethane (160 mL) at room temperature under nitrogen. The mixture was cooled to 0° C. in an ice bath, and 2-(4-methylpiperazin-1-yl)ethanamine (0.395 mL) was added via a syringe. The mixture was stirred for 25 minutes at 0° C., and sodium triacetoxyborohydride (156 mg) was added as a solid. The reaction mixture was stirred for 15 minutes at 0° C., and powdered activated 3 angstrom molecular sieves were added (1.96 g). The reaction mixture was stirred 2 hours at 0° C., and was allowed to stir and warm slowly to room temperature overnight. LC/MS indicated one major peak with a mass that corresponded to desired product. The reaction mixture was quenched with dichloromethane and water. The layers were separated, and aqueous layer was extracted with dichloromethane and 10percent methanol/dichloromethane. The aqueous layer was neutralized with saturated aqueous NaHCO3 mixture, and was extracted one more time with 10percent methanol/dichloromethane. The combined extracts were washed with saturated aqueous NaHCO3 and brine, dried with Na2SO4, filtered, and concentrated. The residue was dissolved in dichloromethane and was purified on a Grace Reveleris X2 MPLC using a Teledyne Isco RediSep? Rf gold 750 g silica gel column eluting with a gradient of 0-20percent of methanol/dichloromethane over 40 minutes. The mixed fractions were purified on a Grace Reveleris X2 MPLC using a Teledyne Isco RediSep? Rf gold 330 g silica gel column eluting with a ramp of 0-15percent of methanol/dichloromethane over 40 minutes to collect additional title compound. The material from both columns was combined to provide the title compound. 1H NMR (501 MHz, dimethyl sulfoxide-d6) delta ppm 8.61 (m, 2H), 7.47 (m, 2H), 7.39 (d, 1H), 7.17 (m, 7H), 7.04 (td, 1H), 6.96 (dd, 1H), 6.67 (d, 1H), 6.51 (d, 1H), 5.84 (dd, 1H), 5.06 (m, 2H), 4.07 (ddq, 2H), 3.90 (d, 1H), 3.75 (s, 3H), 3.68 (dd, 2H), 3.50 (d, 1H), 3.17 (m, 1H), 3.08 (m, 1H), 2.90 (m, 2H), 2.65-2.20 (m, 10H), 2.14 (s, 3H), 1.67 (s, 3H), 1.09 (t, 3H). MS (ESI) m/z 928.4 (M+H)+., 934-98-5

The synthetic route of 934-98-5 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; AbbVie Inc.; AbbVie Deutschland GmbH & Co. KG; Brady, Patrick B.; Braje, Wilfried; Dai, Yujia; Doherty, George A.; Gong, Jane; Jantos, Katja; Ji, Cheng; Judd, Andrew S.; Kunzer, Aaron R.; Lai, Chunqiu; Mastracchio, Anthony; Risi, Roberto M.; Song, Xiaohong; Souers, Andrew J.; Sullivan, Gerard M.; Tao, Zhi-Fu; Teske, Jesse A.; Wang, Xilu; Wendt, Michael D.; Yu, Yiyun; Zhu, Guidong; Penning, Thomas D.; (218 pag.)US2019/55264; (2019); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

934-98-5, 2-(4-Methylpiperazin-1-yl)ethanamine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A 250 mL round bottom flask equipped with a stir bar was charged with Example 1U (1.96 g) and anhydrous dichloromethane (160 mL) at room temperature under nitrogen. The mixture was cooled to 0° C. in an ice bath, and 2-(4-methylpiperazin-1-yl)ethanamine (0.395 mL) was added via a syringe. The mixture was stirred for 25 minutes at 0° C., and sodium triacetoxyborohydride (156 mg) was added as a solid. The reaction mixture was stirred for 15 minutes at 0° C., and powdered activated 3 angstrom molecular sieves were added (1.96 g). The reaction mixture was stirred 2 hours at 0° C., and was allowed to stir and warm slowly to room temperature overnight. LC/MS indicated one major peak with a mass that corresponded to desired product. The reaction mixture was quenched with dichloromethane and water. The layers were separated, and aqueous layer was extracted with dichloromethane and 10percent methanol/dichloromethane. The aqueous layer was neutralized with saturated aqueous NaHCO3 mixture, and was extracted one more time with 10percent methanol/dichloromethane. The combined extracts were washed with saturated aqueous NaHCO3 and brine, dried with Na2SO4, filtered, and concentrated. The residue was dissolved in dichloromethane and was purified on a Grace Reveleris X2 MPLC using a Teledyne Isco RediSep? Rf gold 750 g silica gel column eluting with a gradient of 0-20percent of methanol/dichloromethane over 40 minutes. The mixed fractions were purified on a Grace Reveleris X2 MPLC using a Teledyne Isco RediSep? Rf gold 330 g silica gel column eluting with a ramp of 0-15percent of methanol/dichloromethane over 40 minutes to collect additional title compound. The material from both columns was combined to provide the title compound. 1H NMR (501 MHz, dimethyl sulfoxide-d6) delta ppm 8.61 (m, 2H), 7.47 (m, 2H), 7.39 (d, 1H), 7.17 (m, 7H), 7.04 (td, 1H), 6.96 (dd, 1H), 6.67 (d, 1H), 6.51 (d, 1H), 5.84 (dd, 1H), 5.06 (m, 2H), 4.07 (ddq, 2H), 3.90 (d, 1H), 3.75 (s, 3H), 3.68 (dd, 2H), 3.50 (d, 1H), 3.17 (m, 1H), 3.08 (m, 1H), 2.90 (m, 2H), 2.65-2.20 (m, 10H), 2.14 (s, 3H), 1.67 (s, 3H), 1.09 (t, 3H). MS (ESI) m/z 928.4 (M+H)+., 934-98-5

The synthetic route of 934-98-5 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; AbbVie Inc.; AbbVie Deutschland GmbH & Co. KG; Brady, Patrick B.; Braje, Wilfried; Dai, Yujia; Doherty, George A.; Gong, Jane; Jantos, Katja; Ji, Cheng; Judd, Andrew S.; Kunzer, Aaron R.; Lai, Chunqiu; Mastracchio, Anthony; Risi, Roberto M.; Song, Xiaohong; Souers, Andrew J.; Sullivan, Gerard M.; Tao, Zhi-Fu; Teske, Jesse A.; Wang, Xilu; Wendt, Michael D.; Yu, Yiyun; Zhu, Guidong; Penning, Thomas D.; (218 pag.)US2019/55264; (2019); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

934-98-5,With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.934-98-5,2-(4-Methylpiperazin-1-yl)ethanamine,as a common compound, the synthetic route is as follows.

To a 10 ml RBF containing a magnetic stir bar was added 2-(4- Methylpiperazine-l-yl)ethanamine (143 mg, 1 mmol) in DCM (1 ml). Let stir under argon at room temperature. 1 , 1′-Carbonyldiimidazole (207 mg, 0.5 mmol) was added to the above solution using a spatula. Started forming a white precipitate. TLC on Sipsi2 in 100percent MeOH against the imidazolde indicated a very polar product.Let the solution stir overnight under argon. TLC indicated the completion of the reaction. Extracted the mixture into 25 ml EtOAc. Washed with 2×20 ml of distilled water and 20 ml brine. Combined the desired fractions and dried over anhydrous MgSOphi Filtered and concentrated in vacuo. Dissolved in the minimumamount of EtOAc and reprecipitated from hexanes. Filtered the product as a colorless solid and dried under vacuum to obtain a 69percent yield.eta and 13C NMR in CDCl3 with 2 drops of MeOD. Sample was designated NTF-2006-1-006A1FfNMR (300 MHz, CDCl3) 0.78 (t, J= 7.5 Hz, 3H), 1.08 (m, J= 7.5 Hz, 2H),1.38 (m, J= 7.5 Hz,4H), 1.47 (br s, 4H), 2.27 (s, 3H), 2.47 (br t,4H),2.54 (br t, 4H), 2.60 (t, J=6 Hz, 3H), 3.08 (m, J= 9.0 Hz, 2H), 3.52 (m, J= 5.7 Hz, 2H), 6.89 (d, J= 9.0 Hz, 2H), 7.07 (t, J= 6.9 Hz, IH), 7.28 (t, J= 8.4 Hz, 2H), 7.45 ( br d,J=1.8 Hz, IH), 7.55 (br d, IH) EPO 13C NMR (75 MHz, CDCl3) 14.00, 20,16, 31.32, 36.84, 43.26, 43.36, 46.23,53.07, 55.21, 56.99, 112.96, 115.64, 124.05, 130.44, 132.81, 136.18, 142.79, 142.84, 156.20FABMS 490 (M+H)+ ;HRMS calcd for 024H36N5O4S+ 489.2410 ; found 490.2510

934-98-5 2-(4-Methylpiperazin-1-yl)ethanamine 70284, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; FLYNN, Gary, A.; YOOL, Andrea, J.; MIGLIATI, Elton, Rodrigues; RITTER, Leslie, S.; WO2008/52190; (2008); A2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

934-98-5, 2-(4-Methylpiperazin-1-yl)ethanamine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: Method B: Oxalyl chloride (2 M in CH2Cl2) was added dropwiseto an ice-cooled solution of 2 in dry CH2Cl2 under an argon atmosphere. After 1 h, the ice-bath was removed and the reaction batch was stirred overnight at ambient temperature in an atmosphere of Ar. Subsequently the solvent was evaporated in vacuo and the crude acyl chloride was dissolved in dry DMF and added dropwise to a stirred suspension of amine and K2CO3 in dry DMF at 0 °C. The stirring was continued for 1 h and then at ambient temperature overnight. After 20 h the suspension was filtered, the solvent evaporated, the residue taken up in water and extracted with CH2Cl2. The organic layer was washed with 5percent aqueous NaHCO3 and brine.Then it was dried over anhydrous sodium sulfate, filtered and the solvent was evaporated in vacuo yielding the raw quinoline-4-carboxamides 9?11, which were further purified by column chromatography., 934-98-5

934-98-5 2-(4-Methylpiperazin-1-yl)ethanamine 70284, apiperazines compound, is more and more widely used in various fields.

Reference：
Article; Hochegger, Patrick; Faist, Johanna; Seebacher, Werner; Saf, Robert; Maeser, Pascal; Kaiser, Marcel; Weis, Robert; Bioorganic and Medicinal Chemistry; vol. 25; 7; (2017); p. 2251 – 2259;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

934-98-5, 2-(4-Methylpiperazin-1-yl)ethanamine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,934-98-5

(i) 3-((4-((4-Aminonaphthalen-1-yl)oxy)pyrimidin-2-yl)amino)-5-methoxy-N-(2-(4-methylpiperazin-1-yl)ethyl)benzamideHATU (200 mg, 0.526 mmol) was added to a solution of 3-((4-((4-((tert- butoxycarbonyl)amino)naphthalen-1-yl)oxy)pyrimidin-2-yl)amino)-5-methoxybenzoic acid (see Fyfe, M. C. T. et al., WO 2014/162126; 200 mg, 0.398 mmol), 2-(4-methylpiperazin-1- yl)ethanamine (100 mg, 0.698 mmol) and Hunig’s Base (200 muIota_, 1.145 mmol) in DMF (2 mL). The reaction mixture was stirred at rt for 72h. The reaction mixture was partitioned between water (10 mL) and DCM (20 mL). The organics were separated, dried (MgSCu), filtered and evaporated to give a brown gum. This material was dissolved in IPA (2 mL) and HCI, 6N in IPA (2 mL, 12.00 mmol) was added. The reaction mixture was stirred overnight. The solvent was evaporated and the residue partitioned between sat. NaHCC>3 (10 mL) and DCM (20 mL). The organics were separated, dried (MgSO4), filtered and evaporated to afford the subtitle compound (200 mg) as a tan glass. LCMS m/z 528 (M+H)+(ES+)

The synthetic route of 934-98-5 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; RESPIVERT LIMITED; TOPIVERT PHARMA LIMITED; FYFE, Matthew Colin Thor; THOM, Stephen Malcolm; BAKER, Thomas Matthew; HARBOTTLE, Gareth William; HASIMBEGOVIC, Vedran; RIGBY, Aaron; WO2015/92423; (2015); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics