Category: 39539-66-7

39539-66-7, 4-Methylpiperazine-1-carbonyl chloride is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

The 4′-OH was protected using methyl pipirazine carbonyl chloride (11 mg, 0.054 mMoles) in 2mL DCM, 200 muL Allyl alcohol and pyridine (21 muL) for 2 hours. The product was purified by silica gel column chromatography and Identified by Mass Spec, MS+1 = 654, 39539-66-7

As the paragraph descriping shows that 39539-66-7 is playing an increasingly important role.

Reference：
Patent; MEDAREX, INC.; WO2005/112919; (2005); 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.39539-66-7,4-Methylpiperazine-1-carbonyl chloride,as a common compound, the synthetic route is as follows.

EXAMPLE 4 Sodium hydride (50% dispersion in mineral oil) (0.8 g.) is added to a suspension of 2-(7-methoxy-1,8-naphthyridin-2-yl)-3-hydroxy-isoindolin-1-one (4.63 g.) in anhydrous dimethylformamide (45 cc.), whilst keeping the temperature between 18-20 C. The reaction mixture is stirred for a further 4 hours 30 minutes. A solution of 1-chlorocarbonyl-4-methylpiperazine (2.7 g.) in anhydrous dimethylformamide (25 cc.) is then added over the course of 15 minutes and at a temperature of 20 C. The suspension is stirred for 17 hours at a temperature of about 20 C., and then anhydrous hexamethylphosphotriamide (7 cc.) is added. After 15 minutes, the reaction mixture is poured into ice-water (500 g.). The precipitate is filtered off and washed with water (45 cc.). A product (6.1 g.) is obtained and is recrystallized from diisopropyl ether (1,500 cc.). 2-(7-Methoxy-1,8 -naphthyridin-2-yl)-3-(4-methylpiperazin-1-yl)carbonyloxy-isoindolin-1-one (3 g.), melting at 191 C., is thus obtained. The 2-(7-methoxy-1,8-naphthyridin-2-yl)-3-hydroxy-isoindolin-1-one can be prepared in the following way: Preparation of 2-acetylamino-7-chloro-1,8-naphthyridine, m.p. 251-253 C., according to S.

39539-66-7, 39539-66-7 4-Methylpiperazine-1-carbonyl chloride 3016935, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; Rhone-Poulenc S.A.; US4016274; (1977); 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.39539-66-7,4-Methylpiperazine-1-carbonyl chloride,as a common compound, the synthetic route is as follows.

EXAMPLE 4 Sodium hydride (50% dispersion in mineral oil) (0.8 g.) is added to a suspension of 2-(7-methoxy-1,8-naphthyridin-2-yl)-3-hydroxy-isoindolin-1-one (4.63 g.) in anhydrous dimethylformamide (45 cc.), whilst keeping the temperature between 18-20 C. The reaction mixture is stirred for a further 4 hours 30 minutes. A solution of 1-chlorocarbonyl-4-methylpiperazine (2.7 g.) in anhydrous dimethylformamide (25 cc.) is then added over the course of 15 minutes and at a temperature of 20 C. The suspension is stirred for 17 hours at a temperature of about 20 C., and then anhydrous hexamethylphosphotriamide (7 cc.) is added. After 15 minutes, the reaction mixture is poured into ice-water (500 g.). The precipitate is filtered off and washed with water (45 cc.). A product (6.1 g.) is obtained and is recrystallized from diisopropyl ether (1,500 cc.). 2-(7-Methoxy-1,8 -naphthyridin-2-yl)-3-(4-methylpiperazin-1-yl)carbonyloxy-isoindolin-1-one (3 g.), melting at 191 C., is thus obtained. The 2-(7-methoxy-1,8-naphthyridin-2-yl)-3-hydroxy-isoindolin-1-one can be prepared in the following way: Preparation of 2-acetylamino-7-chloro-1,8-naphthyridine, m.p. 251-253 C., according to S.

39539-66-7, 39539-66-7 4-Methylpiperazine-1-carbonyl chloride 3016935, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; Rhone-Poulenc S.A.; US4016274; (1977); 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.39539-66-7,4-Methylpiperazine-1-carbonyl chloride,as a common compound, the synthetic route is as follows.

EXAMPLE 28 Triethylamine (3.4 cc. equivalent to 2.44 g.), followed by pyridine (15 cc.) are added to a suspension of 2-(7-chloro-1,8-naphthyridin-2-yl)-5-fluoro-3-hydroxy-1-isoindolinone (2 g.) and 4-chlorocarbonyl-1-methyl-piperazine hydrochloride (3.6 g.) in methylene chloride (30 cc.). The suspension obtained is heated to the reflux temperature (55 C) for 1 hour and further 4-chlorocarbonyl-1-methylpiperazine (3.6 g.) and triethylamine (3.4 cc.) are then added. The mixture is further heated to the reflux temperature for 45 minutes. After cooling, methylene chloride (30 cc.) and water (60 cc.) are added. After phase separation, the aqueous layer is extracted with methylene chloride (60 cc.). The organic extracts are dried over anhydrous sodium sulphate. After filtration and concentration, the residue is triturated in water (30 cc.). The precipitate is filtered off and dried in air. The crude product is recrystallized from acetonitrile (64 cc.). The product is filtered off and then washed with isopropyl ether (60 cc.). This gives 2-(7-chloro-1,8-naphthyridin-2-yl)-5-fluoro-3-(4-methylpiperazinyl)-carbonyloxy-1-isoindolinone (0.8 g.) melting at 247-248 C. 2-(7-chloro-1,8-naphthyridin-2-yl)-5-fluoro-3-hydroxy-1-isoindolinone can be prepared in the following manner:

39539-66-7, The synthetic route of 39539-66-7 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Rhone-Poulenc S.A.; US4016274; (1977); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

39539-66-7, 4-Methylpiperazine-1-carbonyl chloride is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

EXAMPLE 1 [1-methyl-4-(N-pyrrolidinocarbonyl)piperazine] In 50 ml of toluene was dissolved 8.1 g (0.05 mole) of 1-methyl-4-chlorocarbonylpiperazine at room temperature and a solution of 10.7 g (0.15 mole) of pyrrolidine in 50 ml of toluene was dropped to the above solution at 0 C. over a period of 30 minutes. The mixture was refluxed for 1 hour to complete the reaction. The reaction mixture was cooled, and the precipitated yellow crystal (pyrrolidine hydrochloride) was removed by filtration. The filtrate was dried with anhydrous sodium sulfate and toluene as the solvent was removed by distillation under reduced pressure to obtain crude 1-methyl-4-(pyrrolidinocarbonyl)piperazine as the distillation residue. The crude product was purified by distillation under reduced pressure to obtain 6.6 g of a pure product having a boiling point of 109.5 to 110.0 C. at 0.5-0.6 mm Hg obs. The yield was 66.9%. The elementary analysis values are as follows: Found: C=61.07%, H=9.89%, N=21.20% Anal. Calcd for C10 H19 N3 O: C=60.87%, H=9.73%, N=21.30%

39539-66-7, The synthetic route of 39539-66-7 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Mitsuitoatsu Chemicals Inc.; US4420481; (1983); 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.39539-66-7,4-Methylpiperazine-1-carbonyl chloride,as a common compound, the synthetic route is as follows.

EXAMPLE 28 Triethylamine (3.4 cc. equivalent to 2.44 g.), followed by pyridine (15 cc.) are added to a suspension of 2-(7-chloro-1,8-naphthyridin-2-yl)-5-fluoro-3-hydroxy-1-isoindolinone (2 g.) and 4-chlorocarbonyl-1-methyl-piperazine hydrochloride (3.6 g.) in methylene chloride (30 cc.). The suspension obtained is heated to the reflux temperature (55 C) for 1 hour and further 4-chlorocarbonyl-1-methylpiperazine (3.6 g.) and triethylamine (3.4 cc.) are then added. The mixture is further heated to the reflux temperature for 45 minutes. After cooling, methylene chloride (30 cc.) and water (60 cc.) are added. After phase separation, the aqueous layer is extracted with methylene chloride (60 cc.). The organic extracts are dried over anhydrous sodium sulphate. After filtration and concentration, the residue is triturated in water (30 cc.). The precipitate is filtered off and dried in air. The crude product is recrystallized from acetonitrile (64 cc.). The product is filtered off and then washed with isopropyl ether (60 cc.). This gives 2-(7-chloro-1,8-naphthyridin-2-yl)-5-fluoro-3-(4-methylpiperazinyl)-carbonyloxy-1-isoindolinone (0.8 g.) melting at 247-248 C. 2-(7-chloro-1,8-naphthyridin-2-yl)-5-fluoro-3-hydroxy-1-isoindolinone can be prepared in the following manner:

39539-66-7, The synthetic route of 39539-66-7 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Rhone-Poulenc S.A.; US4016274; (1977); 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.39539-66-7,4-Methylpiperazine-1-carbonyl chloride,as a common compound, the synthetic route is as follows.

EXAMPLE 28 Triethylamine (3.4 cc. equivalent to 2.44 g.), followed by pyridine (15 cc.) are added to a suspension of 2-(7-chloro-1,8-naphthyridin-2-yl)-5-fluoro-3-hydroxy-1-isoindolinone (2 g.) and 4-chlorocarbonyl-1-methyl-piperazine hydrochloride (3.6 g.) in methylene chloride (30 cc.). The suspension obtained is heated to the reflux temperature (55 C) for 1 hour and further 4-chlorocarbonyl-1-methylpiperazine (3.6 g.) and triethylamine (3.4 cc.) are then added. The mixture is further heated to the reflux temperature for 45 minutes. After cooling, methylene chloride (30 cc.) and water (60 cc.) are added. After phase separation, the aqueous layer is extracted with methylene chloride (60 cc.). The organic extracts are dried over anhydrous sodium sulphate. After filtration and concentration, the residue is triturated in water (30 cc.). The precipitate is filtered off and dried in air. The crude product is recrystallized from acetonitrile (64 cc.). The product is filtered off and then washed with isopropyl ether (60 cc.). This gives 2-(7-chloro-1,8-naphthyridin-2-yl)-5-fluoro-3-(4-methylpiperazinyl)-carbonyloxy-1-isoindolinone (0.8 g.) melting at 247-248 C. 2-(7-chloro-1,8-naphthyridin-2-yl)-5-fluoro-3-hydroxy-1-isoindolinone can be prepared in the following manner:

39539-66-7, The synthetic route of 39539-66-7 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Rhone-Poulenc S.A.; US4016274; (1977); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

39539-66-7, 4-Methylpiperazine-1-carbonyl chloride is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

The 4′-OH was protected using methyl pipirazine carbonyl chloride (11 mg, 0.054 mMoles) in 2mL DCM, 200 muL Allyl alcohol and pyridine (21 muL) for 2 hours. The product was purified by silica gel column chromatography and Identified by Mass Spec, MS+1 = 654, 39539-66-7

As the paragraph descriping shows that 39539-66-7 is playing an increasingly important role.

Reference：
Patent; MEDAREX, INC.; WO2005/112919; (2005); A2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

39539-66-7, 4-Methylpiperazine-1-carbonyl chloride is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

39539-66-7, EXAMPLE 1 4-(5-Chloropyridin-2-yl)-3-methyl-5-[(4-methylpiperazin-1-yl)carbonyl]oxy-1,2,4-triazole 50 g (0.24 mol) of 4-(5-chloropyridin-2-yl)-5-hydroxy-3-methyl-1,2,4-triazole are dissolved or suspended in 1 litre of absolute tetrahydrofuran. The sodium hydride, degreased with toluene, is added thereto from 10.8 g of a 55% sodium hydride dispersion and the mixture is stirred for 1 hour at ambient temperature. Then 39 g (0.24 mol) of freshly distilled 1-chlorocarbonyl-4-methyl-piperazine (Bp17: 120-124 C.) are added dropwise thereto and the mixture is stirred for a further 5 hours whilst moisture is excluded. The resulting suspension is concentrated by evaporation in vacuo and the residue is carefully mixed with water and neutralised. The solution containing the carbamate is extracted several times with methylene chloride and the organic phase is washed with water, dried and concentrated. The residue is triturated with ether and 55 g (68% of theory) of the title compound are obtained in the form of crystals, m.p. 121-122 C. 12.5 g of this base are dissolved in 100 ml of methanol and 4.3 g of fumaric acid are added hot. On cooling, the hemifumarate crystallises out, m.p. 173-175 C. (yield: 17 g). The compound is highly water-soluble; pH of the solution 3.5. The starting compound, 4-(5-chloropyridin-2-yl)-5-hydroxy-3-methyl-1,2,4-triazole, is obtained as follows:

39539-66-7 4-Methylpiperazine-1-carbonyl chloride 3016935, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; Boehringer Ingelheim KG; US4732900; (1988); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

39539-66-7, 4-Methylpiperazine-1-carbonyl chloride is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A solution of this product (50 mg, 0.1 mmol), 4-methylpiperazine-1-carbonylchloride (89 mg, 0.6 mmol), diisopropylethylamine (142 mg, 1.1 mmol), in dioxane (0.5 mL) was submitted to microwave irradiation (300 W) for 60 minutes at 160 C. The reaction solution was cooled to room temperature and slowly poured into a stirring saline solution (10 mL). The resulting precipitate was collected by filtration, washed with water and purified by RP-HPLC (C18, 0 to 100% CH3CN in 0.1% aqueous HCO2H) to yield 1-280 as a pale yellow solid (6 mg, 10%) MS m/z=574 (M+H).

39539-66-7, The synthetic route of 39539-66-7 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Millennium Pharmaceuticals, Inc.; US2005/256102; (2005); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics