Category: 109-01-3

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.109-01-3,1-Methylpiperazine,as a common compound, the synthetic route is as follows.,109-01-3

A mixture of 3-bromopropanol (20 ml), N-methylpiperazine (29 ml), potassium carbonate (83 g) and ethanol (200 ml)was stirred and heated to reflux for 20 hours. The mixture was cooled to ambient temperature and filtered. The filtrate was evaporated and the residue was triturated under diethyl ether. The resultant mixture was filtered and the filtrate was evaporated. The residue was purified by distillation at about 60-70 C. under about 0.2 mm Hg to give 1-(3-hydroxypropyl)-4-methylpiperazine (17 g); NMR Spectrum: (CDCl3) 1.72 (m, 2H), 2.3 (s, 3H), 2.2-2.8 (m, 8H), 2.6 (t, 2H), 3.8 (t, 2H), 5.3 (br s, 1H).

The synthetic route of 109-01-3 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; AstraZeneca AB; US2004/48881; (2004); A1;; ; Patent; Lambert, Christine Marie Paul; Ple, Patrick; US2004/44015; (2004); 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.109-01-3,1-Methylpiperazine,as a common compound, the synthetic route is as follows.

PREPARATION 6 2-(4-Methyl-1-piperazinyl)ethanol 2-Chloroethanol (36.0 g, 30 mL, 0.44 mol) was added to 1-methylpiperazine (27.0 g, 30 mL, 0.27 mol) and potassium carbonate (40 g, 0.29 mol) in acetonitrile (100 mL) with stirring. The reaction mixture was heated under reflux for 48 h, then filtered, and the solids were washed with acetonitrile. The combined filtrates were evaporated under reduced pressure and the resulting oil was distilled at 12 mm Hg to give the title compound (31 g, 0.21 mol) as a light tan oil. Electrospray MS m/z 145 [M+H]+.

109-01-3, The synthetic route of 109-01-3 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Astra Aktiebolag; US6218538; (2001); B1;,
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.109-01-3,1-Methylpiperazine,as a common compound, the synthetic route is as follows.,109-01-3

A mixture of 3-bromopropanol (20 ml), N-methylpiperazine (29 ml), potassium carbonate (83 g) and ethanol (200 ml)was stirred and heated to reflux for 20 hours. The mixture was cooled to ambient temperature and filtered. The filtrate was evaporated and the residue was triturated under diethyl ether. The resultant mixture was filtered and the filtrate was evaporated. The residue was purified by distillation at about 60-70 C. under about 0.2 mm Hg to give 1-(3-hydroxypropyl)-4-methylpiperazine (17 g); NMR Spectrum: (CDCl3) 1.72 (m, 2H), 2.3 (s, 3H), 2.2-2.8 (m, 8H), 2.6 (t, 2H), 3.8 (t, 2H), 5.3 (br s, 1H).

The synthetic route of 109-01-3 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; AstraZeneca AB; US2004/48881; (2004); A1;; ; Patent; Lambert, Christine Marie Paul; Ple, Patrick; US2004/44015; (2004); 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.109-01-3,1-Methylpiperazine,as a common compound, the synthetic route is as follows.

To a solution of 1-(bromomethyl)-4-nitrobenzene (4.0 g, 18.5 mmol) and 1- methylpiperazine (1.7 g, 17.0 mmol) in CH3CN was added K2CO3 (3.8 g, 27.5 mmol), the mixture was stirred at 85 oC overnight. After completion, removed the solvent, extracted with ethyl acetate (150 mL × 3), washed with water (80 mL × 2), brine (80 mL × 2), dried with Na2SO4, purified by silica gel (DCM / MeOH = 50/1, 30/1), light brown solid 1-methyl-4-(4-nitrobenzyl)piperazine (3.3 g) was obtained, yield 76%. LC/MS (ESI) m/z = 236 (M + H) +.

109-01-3, The synthetic route of 109-01-3 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; THE BROAD INSTITUTE, INC.; DANA-FARBER CANCER INSTITUTE, INC.; THE GENERAL HOSPITAL CORPORATION D/B/A MASSACHUSETTS GENERAL HOSPITAL; GRAY, Nathanael, S.; LIANG, Yanke; CHOI, Hwan, Geun; SUNDBERG, Thomas; SHAMJI, Alykhan; XAVIER, Ramnik; FISHER, David E.; (251 pag.)WO2018/9544; (2018); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

109-01-3, 1-Methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

350 ml of ethanol was added to 155 g (1.547 mol) of N-methylpiperazine. At room temperature (25+/-3 C.), 60 g (0.351 mol) of 4-chloromethylbenzoic acid was added thereto and stirred for 6-7 hours. The reaction was analyzed by HPLC, and then the reaction solution was distilled under reduced pressure to remove ethanol, and 60 ml of 1-butanol was added thereto. The mixture was azeotropically distilled at 70+/-2 C. and concentrated to produce a solid. 600 ml of 2-propanol was added thereto and the mixture was stirred at room temperature (25+/-3 C.) for 30 minutes, stirred under reflux for 15 minutes, and then stirred at room temperature (25+/-3 C.) for 12 hours with slow cooling. The produced precipitate was cooled to 19+/-3 C., stirred for 1 hour and then filtered. The filtrate was washed with 50 ml of cooled 2-propanol and dried in an oven at 60 C., thereby obtaining a white compound of formula (2) (60 g, yield: 72%, purity: 95% or higher).HPLC purity: 99.123% (desmethyl impurity: 0.042%, starting material 0.42%).Thin layer chromatography: Methanol-Dichloromethane (7:5), Rf: 0.2., 109-01-3

109-01-3 1-Methylpiperazine 53167, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; BCWORLD PHARM. CO., LTD.; US2012/330014; (2012); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

109-01-3, 1-Methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

350 ml of ethanol was added to 155 g (1.547 mol) of N-methylpiperazine. At room temperature (25+/-3 C.), 60 g (0.351 mol) of 4-chloromethylbenzoic acid was added thereto and stirred for 6-7 hours. The reaction was analyzed by HPLC, and then the reaction solution was distilled under reduced pressure to remove ethanol, and 60 ml of 1-butanol was added thereto. The mixture was azeotropically distilled at 70+/-2 C. and concentrated to produce a solid. 600 ml of 2-propanol was added thereto and the mixture was stirred at room temperature (25+/-3 C.) for 30 minutes, stirred under reflux for 15 minutes, and then stirred at room temperature (25+/-3 C.) for 12 hours with slow cooling. The produced precipitate was cooled to 19+/-3 C., stirred for 1 hour and then filtered. The filtrate was washed with 50 ml of cooled 2-propanol and dried in an oven at 60 C., thereby obtaining a white compound of formula (2) (60 g, yield: 72%, purity: 95% or higher).HPLC purity: 99.123% (desmethyl impurity: 0.042%, starting material 0.42%).Thin layer chromatography: Methanol-Dichloromethane (7:5), Rf: 0.2., 109-01-3

109-01-3 1-Methylpiperazine 53167, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; BCWORLD PHARM. CO., LTD.; US2012/330014; (2012); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

109-01-3, 1-Methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

The First Step: Preparation of 1-methyl-4-(4-nitrobenzyl)-piperazine (F652-01) Monomethylpiperazine (15 mL) and tetrahydrofuran (60 mL) were placed in a 200 mL eggplant shaped flask, and a solution of 4-nitrobenzylchloride (8.58 g, 50 mmol) in tetrahydrofuran was added dropwise to the mixture at room temperature while stirring. After finishing the instillation, the mixture was stirred at room temperature for 24 hours. The reaction mixture was mixed with distilled water, and the precipitated solids were collected by filtration and dried under reduced pressure to obtain the title compound (5.9 g, 50%). LC/MS (Method 3): m/z (ESI, POS): 236[M+H]+; retention time: 1.28 minutes., 109-01-3

As the paragraph descriping shows that 109-01-3 is playing an increasingly important role.

Reference£º
Patent; NIPPON KAYAKU KABUSHIKI KAISHA; EP1857446; (2007); 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.109-01-3,1-Methylpiperazine,as a common compound, the synthetic route is as follows.

STARTING MATERIAL SYNTHETIC EXAMPLE 8 5-amino-2-(4-methylpiperazin-1-yl)benzonitrile By the reaction and treatment in the same manner as in Starting Material Synthetic Example 4 using 2-chloro-5-nitrobenzonitrile (15 g) and methylpiperazine (9.8 g), the title compound (11.1 g) was obtained. melting point: 45-46¡ã C., 109-01-3

The synthetic route of 109-01-3 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Ushio, Hiroyuki; Naito, Youichiro; Sugiyama, Naoki; Kawaguchi, Takafumi; Ohtsuki, Makio; Chiba, Kenji; US2003/203909; (2003); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

109-01-3, 1-Methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Example 5 (Synthesis of 4-[(4-methyl-1-piperazinyl)methyl]benzoic acid 4-(Chloromethyl)benzoic acid (58 g) is added to a solution of N-methylpiperazine (150 g) in n-BuOH (580 g) at room temperature. After stirring for 3-6 h, the solvent is evaporated under reduced pressure and the residue is taken up with IPA (440 g). The mixture is refluxed for 15 min under stirring, then stirred for 24 h at room temperature. The solid is filtered off, washed with IPA (2*58 g) and dried under vacuum at 70 C. overnight. The desired product is obtained as a white solid (59.5 g, 75% yield).

109-01-3, As the paragraph descriping shows that 109-01-3 is playing an increasingly important role.

Reference£º
Patent; MacDonald, Peter; Rossetto, Pierluigi; US2008/103305; (2008); 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.109-01-3,1-Methylpiperazine,as a common compound, the synthetic route is as follows.

A. 1-methyl-4-[(4-nitrophenyl)methyl]piperazine To a solution of p-nitrobenzyl chloride (5.2 g, 10mM) and 3.2 g of triethylamine in 30 ml of ethylene glycol is added a solution of N-methylpiperazine (3 g, 30 mM) in 20 ml of ethylene glycol. After complete addition, the resulting solution is heated to 80 C. under nitrogen for 30 minutes. The reaction mixture is quenched into aqueous 10% sodium carbonate solution and extracted with methylene chloride. The methylene chloride solution is washed with water, saturated sodium chloride solution, dried over anhydrous sodium sulfate and concentrated to give 4.15 g (59%) of 1-methyl-4-[(4-nitrophenyl)methyl]piperazine.

109-01-3, As the paragraph descriping shows that 109-01-3 is playing an increasingly important role.

Reference£º
Patent; The Upjohn Company; US4140775; (1979); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics