Analyzing the synthesis route of Piperazine Dihydrochloride

The synthetic route of 142-64-3 has been constantly updated, and we look forward to future research findings.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.142-64-3,Piperazine Dihydrochloride,as a common compound, the synthetic route is as follows.

Anhydrous piperazine 1 9.5 g (0.11 mol) and piperazinium dihydrochloride 2 31.8 g (0.2 mol) were dissolved in ethanol (80 mL), and the mixture was heated at 75 C for 3 h. To the solution, benzyl chloride 13.9 g (0.11 mol) was added dropwise. The reaction mixture was refluxed for another 2 h monitoring by TLC. The stirring mixture was cooled and then filtered. The filter cake was washed with ethanol and the filtrate was concentrated in vacuo, which was then washed with a solution of NaOH (6 M, pH > 12). The aqueous layer was extracted with CH2Cl2 at pH > 12. The organic layers were combined, dried over Na2SO4, and concentrated in vacuo. The crude product was purified by flash column chromatography on silica gel (1:3 MeOH/CH2Cl2) to give N-benzylpiperazine 3 18.4 g; yield 95 %. 1HNMR (500 MHz, CDCl3): 7.34-7.28 (m, 5H, Ph), 3.57 (s, 2H, OBn), 3.23 (s, 4H, piperazine-H), 2.77 (s, 4H, piperazine-H). MS (ESI): m/z = 176 (M+ +H). Spectroscopic data are according to the literature [19]., 142-64-3

The synthetic route of 142-64-3 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Hu, Xiao; Qiu, Qiong; Wang, Wen-Ling; Wang, Jin; Research on Chemical Intermediates; vol. 43; 1; (2017); p. 57 – 61;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Simple exploration of Piperazine Dihydrochloride

142-64-3 Piperazine Dihydrochloride 8893, apiperazines compound, is more and more widely used in various fields.

142-64-3, Piperazine Dihydrochloride is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: General procedure for the synthesis of compounds (8a, 8b).A solution of anhydrous piperazine (5, 8.6 g, 0.1 mol) and piperazine dihydrochloride (6, 31.8 g 0.2 mol) in ethanol (80 mL) were heated with vigorous stirring at 75 C for 2 h. Then a solution benzylchloride (13.9 g, 0.11 mol) or benzoyl chloride (15.4 g,0.11 mol) was added dropwise over a period of 40 min to the hotsolution. The reaction mixture was refluxed for another 2 h, the progress of the reaction was monitored by TLC. The mixture wascooled and the precipitated piperazine dihydrochloride 6 was collected and washed three times with ethanol. The filtrate combined with the washes was concentrated in vacuo to give the N-benzylpiperazineor N-benzoylpiperazine hydrochloride which was then treated with 6 M NaOH to pH > 12. The aqueous layerof crude N-benzylpiperazine or N-benzoylpiperazine was extractedinto CH2Cl2 (3 50 mL). The combined organic extracts were driedover Na2SO4 and concentrated in vacuo. The crude oily product was purified by flash column chromatography on silica gel (MeOHCH2Cl21:3) to give 8a (18.4 g, 95%) or 8b (17.8 g, 94%)., 142-64-3

142-64-3 Piperazine Dihydrochloride 8893, apiperazines compound, is more and more widely used in various fields.

Reference£º
Article; Wang, Jin; Xia, Fei; Jin, Wen-Bin; Guan, Jin-Yan; Zhao, Hang; Bioorganic Chemistry; vol. 68; (2016); p. 214 – 218;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Downstream synthetic route of Piperazine Dihydrochloride

As the paragraph descriping shows that 142-64-3 is playing an increasingly important role.

142-64-3, Piperazine Dihydrochloride is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

(1) Put the solvent ethanol into the reactor, add piperazine, and stir to dissolve all the piperazine. Hydrochloric acid is added dropwise under the condition of 20 C to make the reaction solution PH = 2 as an end point; after reacting for 1 hour and cooling to 20 C,Pipette rejection by centrifugation to give piperazine dihydrochloride, the mother liquor can continue to be concentrated to give piperazine dihydrochloride;(2) The ethanol into the reaction vessel was added with stirring 42g piperazine dihydrochloride and 21g of piperazine,Reaction at 68 C for 3 hours;(3) cooling to 45 C dropwise cinnamyl chloride 36g, after the dropwise addition was warmed to 60 incubated for 4 hours,And then cooled to 10 C, centrifuged, the solid filter cake was recovered to give piperazine dihydrochloride recycling, the mother liquor drawn into the distillation reactor;(4) heat distillation mother liquor recovery solvent,The solvent is no longer out when adding purified water,Dropping lye to adjust PH to 12,The mixture was extracted with chloroform twice, the organic phases were combined and the organic phase was washed twice with water. The organic phase was separated and dried over anhydrous sodium sulfate overnight. The chloroform was then recovered by distillation and the product was still hot while still in the still pot to give cinnamylpiperazine., 142-64-3

As the paragraph descriping shows that 142-64-3 is playing an increasingly important role.

Reference£º
Patent; Zhengzhou Ruikang Pharmaceutical Co., Ltd.; Zhang Jie; Zhang Guoyong; Li Mingxuan; Liu Yuanyuan; (6 pag.)CN106366051; (2017); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Some tips on Piperazine Dihydrochloride

142-64-3 Piperazine Dihydrochloride 8893, apiperazines compound, is more and more widely used in various fields.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.142-64-3,Piperazine Dihydrochloride,as a common compound, the synthetic route is as follows.

Weigh tert-butylbenzoic acid 9.0g (0.05mol) was dissolved in 20ml of dry tetrahydrofuran was slowly added CDI8.9g (0.055mol), at room temperature for 4hAfter the reaction solution through a dropping funnel was added dropwise to a solution of constant piperazine dihydrochloride 20g (0.125mol), anhydrous piperazine 10g (0.125mol), 60ml of an aqueous solution of sodium chloride, 14g, and reacted for 5 hours at room temperature .After completion of the reaction by suction, the filtrate evaporated to remove THF, 10ml ethyl acetate again, NaOH saturated solution was adjusted to pH = 10, and the combined organic phase was extracted 3 times with ethyl acetate. The organic phase was dried over anhydrous sodium sulfate overnight, pumping filtered, spin dry ethyl acetate, the resulting white crystals is 1- (4-tert-butyl-benzoyl) piperazine crude product 5.9g, 48% yield., 142-64-3

142-64-3 Piperazine Dihydrochloride 8893, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; Xi’an Jiaotong University; Zhang, Jie; Lu, Wen; Dong, Jinyun; Pan, Xiaoyan; He, Langchong; Zhang, Tao; Wang, Sicen; Shen, Xiuxiu; (16 pag.)CN104262238; (2016); B;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Downstream synthetic route of 142-64-3

142-64-3, As the paragraph descriping shows that 142-64-3 is playing an increasingly important role.

142-64-3, Piperazine Dihydrochloride is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Compound, 2 (250 mg, 1.23 mmol) was taken in THF, and piperazinedihydrochloride (199 mg, 1.25 mmol) and K2CO3 (690mg, 5 mmol) were added. The reaction mixture was refluxed overnight.After complete reaction the solvent was removed under reduced pressure and theprecipitate obtained was washed with water and hexane (5 x 3ml). The crudeproduct was purified by column chromatographyusing gradient of ethylacetate andhexane (20 % v/v) to obtain off white color compound. Yield 80 % (250mg). M.p. 91-92C. 1H NMR(300 MHz, CDCl3) delta (ppm): 7.38-7.12 (m, 10 H), 4.21 (s, 1H),2.40 (Br, 8 H).

142-64-3, As the paragraph descriping shows that 142-64-3 is playing an increasingly important role.

Reference£º
Article; Srivastava, Priyanka; Ali, Rashid; Razi, Syed S.; Shahid, Mohammad; Patnaik, Satyakam; Misra, Arvind; Tetrahedron Letters; vol. 54; 28; (2013); p. 3688 – 3693;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Simple exploration of 142-64-3

142-64-3, 142-64-3 Piperazine Dihydrochloride 8893, apiperazines compound, is more and more widely used in various fields.

142-64-3, Piperazine Dihydrochloride is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Weigh between methoxybenzoate 7.6g (0.05mol) was dissolved in 20ml of dry tetrahydrofuran was slowly added CDI8.9g (0.055mol), at room temperature for 4hAfter the reaction solution through a dropping funnel was added dropwise to a solution of constant piperazine dihydrochloride 20g (0.125mol), anhydrous piperazine 10g (0.125mol), 60ml of an aqueous solution of sodium chloride, 14g, and reacted for 5 hours at room temperature .After completion of the reaction by suction, the filtrate evaporated to remove THF, 10ml ethyl acetate again, NaOH saturated solution was adjusted to pH = 10, and the combined organic phase was extracted 3 times with ethyl acetate. The organic phase was dried over anhydrous sodium sulfate overnight, pumping filtered, spin dry ethyl acetate, the resulting white crystals is 1- (3-methoxybenzoyl) piperazine crude product 6.5g, 59% yield.

142-64-3, 142-64-3 Piperazine Dihydrochloride 8893, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; Xi’an Jiaotong University; Zhang, Jie; Lu, Wen; Dong, Jinyun; Pan, Xiaoyan; He, Langchong; Zhang, Tao; Wang, Sicen; Shen, Xiuxiu; (16 pag.)CN104262238; (2016); B;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Brief introduction of 142-64-3

The synthetic route of 142-64-3 has been constantly updated, and we look forward to future research findings.

142-64-3, Piperazine Dihydrochloride is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,142-64-3

EXAMPLE 27 In a 100-ml. flask was placed 1.59 g. of piperazine dihydrochloride and 3 ml. of water. To the resulting solution was added 3.92 g. of 2,3,4-trimethoxybenzaldehyde dissolved in 15 ml. of methanol. A solution of 0.98 g. of sodium cyanide in 5 ml. of water was added dropwise to the mixture over a period of about 10 minutes with ice cooling. Then the reaction mixture, from which crystalline precipitate separated upon heating, was stirred for 2.5 hours while the external temperature was kept at 40 to 50C. After the mixture was cooled, crystal was collected by filtration, washed with water and methanol, and dried. There was obtained 4.3 g. of crystal having a melting point of 244 – 247C. Recrystallization from chloroform-methanol afforded N,N’-bis-(alpha-cyano-2,3,4-trimethoxybenzyl)piperazine as a crystalline product melting at 245 – 247C.

The synthetic route of 142-64-3 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Fuji Chemical Industry Co., Ltd.; Nippon Chemiphar Co., Ltd.; US3962247; (1976); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Some tips on 142-64-3

142-64-3 Piperazine Dihydrochloride 8893, apiperazines compound, is more and more widely used in various fields.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.142-64-3,Piperazine Dihydrochloride,as a common compound, the synthetic route is as follows.

A solution of anhydrous piperazine (1, 9.4 g, 0.11 mol) and piperazine dihydrochloride (2, 31.8 g, 0.20 mol) in ethanol (80 mL) was placed in a three-necked flask equipped with a magnetic stir bar and reflux condenser and was heated with vigorous stirring at 65 C for 3 h. Then benzyl chloride (12.6 g, 0.10 mol) was added dropwise over a period of 45 min to the reaction mixture, which was then refluxed for another 2h. The progress of the reaction was monitored by TLC. The mixture was cooled and the precipitated piperazine dihydrochloride (2) was recovered. The combined filtrate was concentrated under reduced pressure to give the N-benzylpiperazine hydrochloride, which was then treated with 4 M NaOH to pH > 12. The aqueous layer of crude N-benzylpiperazine was extracted with CHCl3 (3 ¡Á 50 mL). The combined organic extracts were dried over Na2SO4 and concentrated under reduced pressure. The crude product was purified by flash column chromatography on silica gel (1:5 MeOH-CH2Cl2) to give 4: Yield 18.3 g (95%); 1H NMR (500 MHz, CDCl3): delta 7.34-7.28 (m, 5H),3.57 (s, 2H), 3.23 (s, 4H), 2.77 (s, 4H); MS (ESI) m/z: 177 [M + H]+.Spectroscopic data are according to the literature.13, 142-64-3

142-64-3 Piperazine Dihydrochloride 8893, apiperazines compound, is more and more widely used in various fields.

Reference£º
Article; Hu, Xiao; Chen, Hui; Wu, Wei-Jun; Wang, Wen-Ling; Wang, Jin; Journal of Chemical Research; vol. 40; 9; (2016); p. 519 – 520;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Downstream synthetic route of 142-64-3

As the paragraph descriping shows that 142-64-3 is playing an increasingly important role.

142-64-3, Piperazine Dihydrochloride is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: General procedure for the synthesis of compounds (8a, 8b).A solution of anhydrous piperazine (5, 8.6 g, 0.1 mol) and piperazine dihydrochloride (6, 31.8 g 0.2 mol) in ethanol (80 mL) were heated with vigorous stirring at 75 C for 2 h. Then a solution benzylchloride (13.9 g, 0.11 mol) or benzoyl chloride (15.4 g,0.11 mol) was added dropwise over a period of 40 min to the hotsolution. The reaction mixture was refluxed for another 2 h, the progress of the reaction was monitored by TLC. The mixture wascooled and the precipitated piperazine dihydrochloride 6 was collected and washed three times with ethanol. The filtrate combined with the washes was concentrated in vacuo to give the N-benzylpiperazineor N-benzoylpiperazine hydrochloride which was then treated with 6 M NaOH to pH > 12. The aqueous layerof crude N-benzylpiperazine or N-benzoylpiperazine was extractedinto CH2Cl2 (3 50 mL). The combined organic extracts were driedover Na2SO4 and concentrated in vacuo. The crude oily product was purified by flash column chromatography on silica gel (MeOHCH2Cl21:3) to give 8a (18.4 g, 95%) or 8b (17.8 g, 94%).Data for 8a [21]: 1H NMR (500 MHz, CDCl3): 7.34-7.28 (m, 5H,Ph), 3.57 (s, 2H, OBn), 3.23 (s, 4H, piperazine-H), 2.77 (s, 4H,piperazine-H). MS (ESI): m/z = 177 [M + H]+. Spectroscopic dataare according to the literature [21].Data for 8b [22]: 1H NMR (500 MHz, CDCl3): 7.40 (s, 5H, Ph-H),3.78 (s, 2H), 3.42 (s, 2H), 2.40-3.10 (m, 5H). MS (ESI): m/z = 191 [M+ H]+. Spectroscopic data are according to the literature [22]., 142-64-3

As the paragraph descriping shows that 142-64-3 is playing an increasingly important role.

Reference£º
Article; Wang, Jin; Xia, Fei; Jin, Wen-Bin; Guan, Jin-Yan; Zhao, Hang; Bioorganic Chemistry; vol. 68; (2016); p. 214 – 218;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Brief introduction of 142-64-3

142-64-3, The synthetic route of 142-64-3 has been constantly updated, and we look forward to future research findings.

142-64-3, Piperazine Dihydrochloride is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Weigh 2,4-dichlorobenzoic acid 9.6g (0.05mol) was dissolved in 20ml of dry tetrahydrofuran was slowly added CDI8.9g (0.055mol), at room temperature for 4hAfter the reaction solution through a dropping funnel was added dropwise to a solution of constant piperazine dihydrochloride 20g (0.125mol), anhydrous piperazine 10g (0.125mol), 60ml of an aqueous solution of sodium chloride, 14g, and reacted for 5 hours at room temperature .After completion of the reaction by suction, the filtrate evaporated to remove THF, 10ml ethyl acetate again, NaOH saturated solution was adjusted to pH = 10, and the combined organic phase was extracted 3 times with ethyl acetate. The organic phase was dried over anhydrous sodium sulfate overnight, pumping filtered, spin dry ethyl acetate, the resulting white crystals is 1- (2,4-dichloro-benzoyl) piperazine crude product 5.8g, 45% yield.

142-64-3, The synthetic route of 142-64-3 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Xi’an Jiaotong University; Zhang, Jie; Lu, Wen; Dong, Jinyun; Pan, Xiaoyan; He, Langchong; Zhang, Tao; Wang, Sicen; Shen, Xiuxiu; (16 pag.)CN104262238; (2016); B;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics