Category: 300543-56-0

300543-56-0, (R)-1-((4-Chlorophenyl)(phenyl)methyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

2 g of R-I- ( (4-chlorophenyl) (phenyl) methyl) piperazine and 0.88 g of diglycolic acid anhydride were dissolved in 10 ml of dimethylsulphoxide . To the solution 20 ml of tetrabutylammo- nium bromide were added. The solution was stirred for another 10 hours until the reaction was completed. The solution was diluted with 67 ml of water and 15 ml of isopropyl acetate were added. The phases were separated and the water layer was reextracted with isopropyl acetate. The organic layer was mixed with demineralised water (40 ml) and the pH of the suspension was adjusted to 10 with 2 M NaOH. The layers were separated and to the water phase 40 ml of isopropyl acetate were added. The pH of the suspension was adjusted to 3.5. The layers were separated and the water phase was reextracted twice with isopropylacetate . The organic phase was rinsed with water and evaporated to dryness. 2.5 g of product (HPLC (area) was 98.5 %) ) was crystallised. The product was dried at vacuum at 500C., 300543-56-0

As the paragraph descriping shows that 300543-56-0 is playing an increasingly important role.

Reference：
Patent; KRKA, tovarna zdravil, d.d., Novo Mesto; WO2009/150147; (2009); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

300543-56-0, (R)-1-((4-Chlorophenyl)(phenyl)methyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,300543-56-0

Example 3; Preparation of oxalate salt of Compound (III); A solution of compound (III, obtained above) in IPA (508 ml) was heated to 40-45C. To this, oxalic acid (78.13 g) was added. The reaction mixture was allowed to reflux to 80-85C for 30 min and then cooled at 20-30C and stirred for 5h. The solid thus obtained was filtered and washed with IPA (124 ml). The title compound was then dried under vacuum at 50-55 C for 12h. The title compound (1 15.0 g) was obtained with 71.65% yield.

As the paragraph descriping shows that 300543-56-0 is playing an increasingly important role.

Reference：
Patent; JUBILANT LIFE SCIENCES LIMITED; BISWAS, Sujay; DUBEY, Shailendra, Kumar; MANGLA, Amit; MASAND, Mukesh; VIR, Dharam; WO2012/101475; (2012); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

300543-56-0, (R)-1-((4-Chlorophenyl)(phenyl)methyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Alternative A2 g of R-I- ( (4-chlorophenyl) (phenyl) methyl) piperazine and 0.88 g of diglycolic acid anhydride was dissolved in 107 mL of acetonitrile . The reaction mixture was refluxed for 12 h. After the reaction was completed the solvent was evaporated and the obtained residue dissolved in 20 mL water with addition of 2mL of IM NaOH and then 10 mL of dichloromethane was added. The suspension was stirred for 20 minutes and the organic phase was separated. To the aqueous phase another portion of 10 mL of dichloromethane was added, pH of suspension is adjusted at 4.5 to 5. Aqueous phase was extracted twice again with 2xl0mL of dichloromethane. Organic phases were collected, dried over anhydrous sodium sulfate, filtrated and evaporated. The obtained crude product could be used in the next step without further purification., 300543-56-0

The synthetic route of 300543-56-0 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; KRKA, TOVARNA ZDRAVIL, D.D., NOVO MESTO; WO2008/110586; (2008); A2;,
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.300543-56-0,(R)-1-((4-Chlorophenyl)(phenyl)methyl)piperazine,as a common compound, the synthetic route is as follows.

General procedure: The title compound was prepared according to General Protocol B. NMR (400 MHz, DMSO-c delta 7.48 – 7.14 (m, 9H), 4.29 (s, 1 H), 2.38 (s, 4H), 2.34 – 2.20 (m, 6H); LCMS ti (Method 1) = 4.630 min, m/z 317.2 [M+H+].General Protocol B. A solution of amine (0.105 mmol) in MeOH (1.00 mL) was treated at room temperature with aldehyde (0.525 mmol to 1.05 mmol, 5.0 to 10.0 equiv.), NaCNBH4 (19.7 mg, 0.315 mmol, 3.0 equiv.) and acetic acid (0.018 mL, 0.315 mmol, 3.0 mmol). The reaction mixture was stirred at room temperature for 1 – 8 h and quenched with 1 N NaOH solution. The mixture was dried by blowing air, re-dissolved in DMSO, filtered and purified by HPLC. The title compound was prepared according to General Protocol B as a TFA salt. LCMS t, (Method 1) = 3.990 min, m/z 445.2 [M+H+]., 300543-56-0

As the paragraph descriping shows that 300543-56-0 is playing an increasingly important role.

Reference：
Patent; THE UNITED STATES OF AMERICA, AS REPRESENTED BY THE SECRETARY, DEPARTMENT OF HEALTH AND HUMAN SERVICES; LIANG, Tsanyang Jake; FERRER, Marc; HE, Shanshan; HU, Xin; HU, Zongyi; MARUGAN, Juan Jose; SOUTHALL, Noel Terrence; XIAO, Jingbo; ZHENG, Wei; WO2015/80949; (2015); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

300543-56-0, (R)-1-((4-Chlorophenyl)(phenyl)methyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A mixture containing (4-chlorophenyl)phenyl methylamine free base (4.1 g, 18.8 mmol), N,N-bis(2-chloroethyl) 4-nitrophenyl carbamate (6.4 g, 20.8 mmol) potassium iodide (1.7 g, 10 mmol) and diisopropyl ethylamine (10.2 ml) was stirred at 140 C. (oil bath) for 4 hours.While cooling down, 60 ml dichloromethane was added. The mixture was stirred at ambient temperature for 20 min. 30 ml HCl (1M) was added to the dichloromethane. The organic layer was separated washed with NaCl (5 ml) dried and concentrated to give an oily material (13.6 g).Above crude material was dissolved in a solution containing 5.3 g NaOH in 10 ml H2O and 42 ml 2-propanol. The mixture was heated til 50 C. for 3 h 30 min.The mixture was concentrated in vacuo to get rid of 2-propanol and redissolved in 40 ml toluene and 20 ml H2O. The mixture was stirred for 30 min, the solid was filtered off and layers were separated. 40 ml HCl (2M) was added to the toluene layer and stirred for 20 min. Separated toluene layer was extracted again with 40 ml HCl (1M). Acidic layers were combined, washed with 40 ml toluene and basified. The mixture was extracted with toluene (80 ml). The separated organic layer was washed with H2O (10 ml), NaCl (10 ml) dried and concentrated in vacuo to give the desired product (1.2 g oil). To the crude product ethyl acetate (25 ml) was added, followed by addition of 0.9 g oxalic acid dissolved in 2 ml EtOH. Suspension was stirred 4 h at ambient temperature and overweekend at 5 C. Solid obtained was filtered off and dried at air to give a solid material (1.3 g, 17.6% yield). 98.56% ee purity., 300543-56-0

The synthetic route of 300543-56-0 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Zhu, Jie; US2009/143582; (2009); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

300543-56-0, (R)-1-((4-Chlorophenyl)(phenyl)methyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A mixture containing (4-chlorophenyl)phenyl methylamine free base (4.1 g, 18.8 mmol), N,N-bis(2-chloroethyl) 4-nitrophenyl carbamate (6.4 g, 20.8 mmol) potassium iodide (1.7 g, 10 mmol) and diisopropyl ethylamine (10.2 ml) was stirred at 140 C. (oil bath) for 4 hours.While cooling down, 60 ml dichloromethane was added. The mixture was stirred at ambient temperature for 20 min. 30 ml HCl (1M) was added to the dichloromethane. The organic layer was separated washed with NaCl (5 ml) dried and concentrated to give an oily material (13.6 g).Above crude material was dissolved in a solution containing 5.3 g NaOH in 10 ml H2O and 42 ml 2-propanol. The mixture was heated til 50 C. for 3 h 30 min.The mixture was concentrated in vacuo to get rid of 2-propanol and redissolved in 40 ml toluene and 20 ml H2O. The mixture was stirred for 30 min, the solid was filtered off and layers were separated. 40 ml HCl (2M) was added to the toluene layer and stirred for 20 min. Separated toluene layer was extracted again with 40 ml HCl (1M). Acidic layers were combined, washed with 40 ml toluene and basified. The mixture was extracted with toluene (80 ml). The separated organic layer was washed with H2O (10 ml), NaCl (10 ml) dried and concentrated in vacuo to give the desired product (1.2 g oil). To the crude product ethyl acetate (25 ml) was added, followed by addition of 0.9 g oxalic acid dissolved in 2 ml EtOH. Suspension was stirred 4 h at ambient temperature and overweekend at 5 C. Solid obtained was filtered off and dried at air to give a solid material (1.3 g, 17.6% yield). 98.56% ee purity., 300543-56-0

The synthetic route of 300543-56-0 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Zhu, Jie; US2009/143582; (2009); 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.300543-56-0,(R)-1-((4-Chlorophenyl)(phenyl)methyl)piperazine,as a common compound, the synthetic route is as follows.

Example 5; Preparation of Compound (II) & its hydrochloride salt; Compound III (obtained in example 2) was taken in toluene (300 ml). To this, 2-chloroethanol (23.29 g) and triethylamine (72.12 ml) were added and then heated to 1 10-1 15C for 3h. After cooling the reaction mass to 75-80C, the remaining 15.52 g of 2-chloroethanol was added. The temperature of the reaction mixture was further raised to 1 10-1 15C and maintained at this temperature for 4h. The progress of reaction was montiored by HPLC. After the completion, it was allowed to cool to 25- 30C and followed by the addition of water (150 ml) and stirred for 10 min. After separating the organic layer, it was washed with water (75ml) and then 1 12.5 ml of water was added to the organic layer. The pH of the reaction mixture was adjusted to 1.0-2.0 using cone. HC1 (~28 ml). After stirring, the aqueous layer was separated. To the aqueous layer, dichloromethane (225 ml) was added and adjusted the pH to 9.5- 10.0 using liquid ammonia. The organic layer was separated, washed with water (150 ml) and concentrated to yield an oily mass of title compound. This oily mass was taken in acetone (750 ml) and heated at 40-45C to get clear solution. The reaction mixture was cooled to 25-30C and cone. HC1 (45.8 ml) was added. It was allowed to stir for 12h at 25-30C. The solid thus obtained was washed with acetone (75 ml) and dried under vacuum to yield 68.61 g hydrochloride salt of title compound with 49.4% yield (with respect to compound (V)).

300543-56-0, The synthetic route of 300543-56-0 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; JUBILANT LIFE SCIENCES LIMITED; BISWAS, Sujay; DUBEY, Shailendra, Kumar; MANGLA, Amit; MASAND, Mukesh; VIR, Dharam; WO2012/101475; (2012); 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.300543-56-0,(R)-1-((4-Chlorophenyl)(phenyl)methyl)piperazine,as a common compound, the synthetic route is as follows.

Example 5; Preparation of Compound (II) & its hydrochloride salt; Compound III (obtained in example 2) was taken in toluene (300 ml). To this, 2-chloroethanol (23.29 g) and triethylamine (72.12 ml) were added and then heated to 1 10-1 15C for 3h. After cooling the reaction mass to 75-80C, the remaining 15.52 g of 2-chloroethanol was added. The temperature of the reaction mixture was further raised to 1 10-1 15C and maintained at this temperature for 4h. The progress of reaction was montiored by HPLC. After the completion, it was allowed to cool to 25- 30C and followed by the addition of water (150 ml) and stirred for 10 min. After separating the organic layer, it was washed with water (75ml) and then 1 12.5 ml of water was added to the organic layer. The pH of the reaction mixture was adjusted to 1.0-2.0 using cone. HC1 (~28 ml). After stirring, the aqueous layer was separated. To the aqueous layer, dichloromethane (225 ml) was added and adjusted the pH to 9.5- 10.0 using liquid ammonia. The organic layer was separated, washed with water (150 ml) and concentrated to yield an oily mass of title compound. This oily mass was taken in acetone (750 ml) and heated at 40-45C to get clear solution. The reaction mixture was cooled to 25-30C and cone. HC1 (45.8 ml) was added. It was allowed to stir for 12h at 25-30C. The solid thus obtained was washed with acetone (75 ml) and dried under vacuum to yield 68.61 g hydrochloride salt of title compound with 49.4% yield (with respect to compound (V)).

300543-56-0, The synthetic route of 300543-56-0 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; JUBILANT LIFE SCIENCES LIMITED; BISWAS, Sujay; DUBEY, Shailendra, Kumar; MANGLA, Amit; MASAND, Mukesh; VIR, Dharam; WO2012/101475; (2012); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

300543-56-0, (R)-1-((4-Chlorophenyl)(phenyl)methyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

The title compound also can be prepared by chemical synthesis. A solution of (R)- l-((4-chlorophenyl)(phenyl)methyl)piperazine (50.0 mg, 0.174 mmol) in THF (1.00 mL) and water (0.50 mL) was treated at room temperature with NaOH (6.97 mg, 0.174 mmol) and Mel (10.9 mu, 0.174 mmol). The reaction mixture was stirred at 65 C for 2 h. The reaction mixture was cooled to room temperature. The organic layer was separated, dried, concentrated and purified by Biotage on Si02 with 0-20% of MeOH in CH2C12 to give the title compound as a white solid. LCMS t2 (Method 2) = 3.070 min; m 301.1 [M+H+].

300543-56-0, 300543-56-0 (R)-1-((4-Chlorophenyl)(phenyl)methyl)piperazine 668697, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; THE UNITED STATES OF AMERICA, AS REPRESENTED BY THE SECRETARY, DEPARTMENT OF HEALTH AND HUMAN SERVICES; LIANG, Tsanyang Jake; FERRER, Marc; HE, Shanshan; HU, Xin; HU, Zongyi; MARUGAN, Juan Jose; SOUTHALL, Noel Terrence; XIAO, Jingbo; ZHENG, Wei; WO2015/80949; (2015); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

300543-56-0, (R)-1-((4-Chlorophenyl)(phenyl)methyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

The title compound also can be prepared by chemical synthesis. A solution of (R)- l-((4-chlorophenyl)(phenyl)methyl)piperazine (50.0 mg, 0.174 mmol) in THF (1.00 mL) and water (0.50 mL) was treated at room temperature with NaOH (6.97 mg, 0.174 mmol) and Mel (10.9 mu, 0.174 mmol). The reaction mixture was stirred at 65 C for 2 h. The reaction mixture was cooled to room temperature. The organic layer was separated, dried, concentrated and purified by Biotage on Si02 with 0-20% of MeOH in CH2C12 to give the title compound as a white solid. LCMS t2 (Method 2) = 3.070 min; m 301.1 [M+H+].

300543-56-0, 300543-56-0 (R)-1-((4-Chlorophenyl)(phenyl)methyl)piperazine 668697, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; THE UNITED STATES OF AMERICA, AS REPRESENTED BY THE SECRETARY, DEPARTMENT OF HEALTH AND HUMAN SERVICES; LIANG, Tsanyang Jake; FERRER, Marc; HE, Shanshan; HU, Xin; HU, Zongyi; MARUGAN, Juan Jose; SOUTHALL, Noel Terrence; XIAO, Jingbo; ZHENG, Wei; WO2015/80949; (2015); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics