Some tips on 142-64-3

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.

100 g (1.2 mol) of anhydrous piperazine and 240 g (1.5 mol) of piperazine dihydrochloride were heated to 120 C.160 g (1.2 mol) of 1-[((2-chloroethoxy)ethoxy)ethanol was added dropwise, and heating and stirring were continued after the addition.The temperature was raised to 136-140 C for 1 hour, and TLC showed that the reaction was stopped and the heating was stopped.When the temperature drops to 80 degrees Celsius, add 500 ml of 95% ethanol and cool in the refrigerator overnight.Piperazine dihydrochloride was recovered by filtration the next day, the filter cake was washed well with a small amount of ethanol, and the filtrate was combined.Adding 200 g of 30% sodium hydroxide solution to alkalization, filtering out the insoluble inorganic salts;After removing the solvent by concentration, the residue was extracted with ethyl acetate, and dried hydrogen chloride gas was passed.Filtration and drying gave 1-[((2-hydroxyethoxy)ethoxy)ethyl]piperazine hydrochloride as a white solid; the solid content was over 98%.After recrystallization from a 90% aqueous solution of ethanol, 230 g of white crystals can be obtained in a yield of 72%.The content can reach more than 99.5%.

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

Reference£º
Patent; Nanjing Haiyan Bio-pharmaceutical Technology Co., Ltd.; Bu Gonggaofamingren; (4 pag.)CN109384745; (2019); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Some tips on 142-64-3

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.

100 g (1.2 mol) of anhydrous piperazine and 240 g (1.5 mol) of piperazine dihydrochloride were heated to 120 C.160 g (1.2 mol) of 1-[((2-chloroethoxy)ethoxy)ethanol was added dropwise, and heating and stirring were continued after the addition.The temperature was raised to 136-140 C for 1 hour, and TLC showed that the reaction was stopped and the heating was stopped.When the temperature drops to 80 degrees Celsius, add 500 ml of 95% ethanol and cool in the refrigerator overnight.Piperazine dihydrochloride was recovered by filtration the next day, the filter cake was washed well with a small amount of ethanol, and the filtrate was combined.Adding 200 g of 30% sodium hydroxide solution to alkalization, filtering out the insoluble inorganic salts;After removing the solvent by concentration, the residue was extracted with ethyl acetate, and dried hydrogen chloride gas was passed.Filtration and drying gave 1-[((2-hydroxyethoxy)ethoxy)ethyl]piperazine hydrochloride as a white solid; the solid content was over 98%.After recrystallization from a 90% aqueous solution of ethanol, 230 g of white crystals can be obtained in a yield of 72%.The content can reach more than 99.5%.

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

Reference£º
Patent; Nanjing Haiyan Bio-pharmaceutical Technology Co., Ltd.; Bu Gonggaofamingren; (4 pag.)CN109384745; (2019); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Simple exploration of 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

100 g (1.2 mol) of anhydrous piperazine and 240 g (1.5 mol) of piperazine dihydrochloride were heated to 120 C, 110 g (1.2 mol) of 2-chloroethanol was added dropwise, and heating and stirring were continued after the addition.Warm up to 136-140 degrees Celsius for 1 hourTLC showed that the reaction was stopped and the heating was stopped. When the temperature dropped to 80 degrees Celsius, add 500 ml of 95% ethanol, cool in the refrigerator overnight, the piperazine dihydrochloride was recovered by filtration the next day, the filter cake was washed thoroughly with a small amount of ethanol, the filtrate was combined, and 30% sodium hydroxide solution was added. 200 g of alkalized, filtered off the insoluble inorganic salt; after removing the solvent by concentration, the residue was extracted with ethyl acetate, and dried hydrogen chloride gas was introduced.After filtration and drying, a white solid 1-(2-hydroxyethyl)piperazine hydrochloride was obtained;The solids content is already above 98%. After recrystallization from a 90% aqueous solution of ethanol, 180 g of white crystals can be obtained, the yield is 85%, and the content can reach 99.5% or more., 142-64-3

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

Reference£º
Patent; Wuxi Qianhao Bio-pharmaceutical Co., Ltd.; Peng Haiyan; (4 pag.)CN109400548; (2019); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Analyzing the synthesis route of 142-64-3

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.

3 mmol of piperazine dihydrochloride hydrate was added of 10 mL of CH3CN, TEA (6 mmol) and 2-chloro-3-nitropyridine (1 mmol). After 2 h, at reflux, the mixture was evaporated under reduced pressure and the residue was treated with H2O (5mL) and ethylacetate (5 mL). The aqueous phase was separated and extracted twice with ethylacetate (2¡Á5 mL). The combined organic phases were dried on Na2SO4, filtered and evaporated under reduced pressure. The crude residue was purified by silica gel column chromatography, using dichloromethane/methanol (9:1) as eluent. Yield 62%, as yellow solid. 1H NMR (DMSO-d6): 8.44 (dd, 1H, J=4.5 Hz, J=1.6 Hz), 8.29 (dd, 1H, J=8.1 Hz, J=1.6 Hz), 6.94 (dd, 1H, J=8.1 Hz, J=4.5 Hz), 3.56 (m, 4H), 2.80 (m, 4H)., 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; Moraca, Francesca; De Vita, Daniela; Pandolfi, Fabiana; Di Santo, Roberto; Costi, Roberta; Cirilli, Roberto; D’Auria, Felicia Diodata; Panella, Simona; Palamara, Anna Teresa; Simonetti, Giovanna; Botta, Maurizio; Scipione, Luigi; European Journal of Medicinal Chemistry; vol. 83; (2014); p. 665 – 673;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

New learning discoveries about 142-64-3

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

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.

EXAMPLE 26 In a 300-ml. three necked flask was placed 4.9 g. of sodium cyanide and 10 ml. of water to obtain a homogeneous solution. To the resuting solution was added 16.6 g. of 3,4-dimethoxybenzaldehyde dissolved in 40 ml. of methanol and then a solution of 9.7 g. of piperazine hexahydrate and 7.95 g. of piperazine dihydrochloride in 30 ml. of water. The reaction mixture, from which crystalline precipitate separated upon heating, was stirred for about 1 hour at 60C. After the mixture was cooled, crystal to separate was collected by filtration, washed with water and methanol, and dried. There was obtained 22.8 g. of crystal having a melting point of 216 -218.5C. Recrystallization from chloroform-methanol afforded N,N’-bis-(alpha-cyano-3,4-dimethoxybenzyl)piperazine as a crystalline product melting at 216 -218C., 142-64-3

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

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

New learning discoveries about 142-64-3

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

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 between dimethylaminobenzoate 8.26g (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 N, N- dimethyl-3- (piperazin-1-yl-carbonyl) aniline crude product 6.4g, 55% yield., 142-64-3

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

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

General procedure: 5.1.5 1-[3-(Trifluoromethyl)benzoyl]piperazine (8a) A solution of 3-(trifluoromethyl)benzoic acid (9.5 g, 0.05 mol) and CDI (8.90 g, 0.055 mol) was stirred in 30 ml anhydrous THF at room temperature for 30 min. In a separate round bottom flask added piperazine (10.76 g, 0.125 mol) and piperazine dihydrochloride (20 g, 0.125 mol) in 60 ml of water. The reaction mixture was stirred for 5 min and added 14 g NaCl. Then add the brine solution to the round bottom flask containing acyl imidazole and stir the reaction mixture for 5 h. The mixture was filtered and the filtrate distilled by rotary evaporation to remove THF. The aqueous layer was washed with ethyl acetate (3 * 10 ml) to remove diacylated product. The pH of the aqueous layer was adjusted to about 9 using saturated solution of NaOH and washed with ethyl acetate (4 * 30 ml). The organic layer was washed with water (4 * 25 ml), dried over anhydrous Na2SO4 for overnight, concentrated by rotary evaporation and purified by flash chromatography to afford 1-[3-(trifluoromethyl) benzoyl]piperazine as colorless solid (6.5 g, 50%). The intermediate compounds 1-(3-fluorobenzoyl)piperazine (8b), 1-(3-methoxybenzoyl)piperazine (8c), 1-(4-tert-butylbenzoyl)piperazine (8d), N,N-dimethyl-3-(piperazin-1-ylcarbonyl)aniline (8e), 1-(4-bromobenzoyl) piperazine (8f) and 1-(2,4-dichlorobenzoyl) piperazine (8g) were prepared by commercially available materials 3-fluorobenzoic acid, 3-methoxybenzoic acid, 4-tert-butylbenzoic acid, 3-(dimethylamino) benzoic acid, 4-bromobenzoic acid and 2,4-dichlorobenzoic acid respectively using the similar procedure of 1-[3-(trifluoromethyl)benzoyl]piperazine (8a) described above., 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; Dong, Jinyun; Pan, Xiaoyan; Wang, Jinfeng; Su, Ping; Zhang, Lin; Wei, Fen; Zhang, Jie; European Journal of Medicinal Chemistry; vol. 101; (2015); p. 780 – 789;,
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

100 g (1.2 mol) of anhydrous piperazine and 240 g (1.5 mol) of piperazine dihydrochloride were heated to 120 C.110 g (1.2 mol) of 2-chloroethanol was added dropwise, and heating and stirring were continued after the addition.The temperature was raised to 136-140 C for 1 hour, and TLC showed that the reaction was stopped and the heating was stopped.When the temperature drops to 80 degrees Celsius, add 500 ml of 95% ethanol and cool in the refrigerator overnight.Piperazine dihydrochloride was recovered by filtration the next day, the filter cake was washed well with a small amount of ethanol, and the filtrate was combined.Adding 200 g of 30% sodium hydroxide solution to alkalization, filtering out the insoluble inorganic salts;After the solvent was removed by concentration, the residue was evaporated to ethylamine.The solid content has beenMore than 98%.After recrystallization from a 90% aqueous solution of ethanol, 180 g of white crystals can be obtained in a yield of 85%.The content can reach more than 99.5%., 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; Nanjing Haiyan Bio-pharmaceutical Technology Co., Ltd.; Bu Gonggaofamingren; (4 pag.)CN109384742; (2019); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

New learning discoveries about 142-64-3

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

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.

100g of concentrated hydrochloric acid (12mol / L) 250ml round bottom flask was placed in an ice bath, was slowly added 40g of anhydrous piperazine, the addition, the ice bath was removed, the reaction overnight at room temperature, filtered off with suction, the filter cake was placed It was dried in an oven, the resulting white solid, a piperazine dihydrochloride. o-fluorobenzoic acid was weighed 7g (0.05mol) dissolved in 20ml of dry tetrahydrofuran, was slowly added CDI 8.9g (0.055mol), after 4h the reaction was reacted at room temperature 4 h. Then a constant pressure dropping funnel was added dropwise a solution of piperazine dihydrochloride hydrochloride 20g (0.125mol), anhydrous piperazine 10g (0.125mol), 60ml of 14g of sodium chloride at room temperature after 5 hours the reaction solution is suction filtered, the filtrate was evaporated to dryness to remove THF, extracted with ethyl acetate again 10ml, NaOH saturated solution was adjusted to pH 10, and extracted 3 times with ethyl acetate and the combined organic phases, the organic phase was dried over anhydrous sodium sulfate overnight, filtration, rotary evaporation of ethyl acetate, the resulting white crystals which was 1- (2-fluorophenyl formyl) piperazine The crude product 4.7g, 45% yield.

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

Reference£º
Patent; XI’AN JIAOTONG UNIVERSITY; ZHANG, JIE; ZHANG, TAO; DONG, JINYUN; PAN, XIAOYAN; HE, LANGCHONG; LU, WEN; WANG, SICEN; SHI, YALING; (19 pag.)CN104262263; (2017); B;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

New learning discoveries about 142-64-3

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

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.

To a cooled solution of imidazole at 000 (1.00 g, 14.7 mmol, 2equiv) in 0H2012 (18 mL),benzyl chloroformate (1.03 mL, 7.35 mmol, 1 equiv) was slowly added. After 1h45 ofstirring the white solid (imidazole hydrochloride) was filtered off. The obtained filtrate wasconcentrated, and then solubilised in ethanol (17.5 mL). In another flask the solution ofpiperazine dihydrochloride (1.75 g, 11.03 mmol, 1.5 equiv) in water (17.5 mL) wasprepared, then added dropwisely to ethanolic solution of Cbz-imidazole. The resultedmixture was stirred for 4h30 at room temperature and then concentrated to 1h of itsvolume. Obtained aqueous phase was extracted with chloroform (4x) to remove the diacylated product, then NaOHsat was added to the previous aqueous phase (pH 9-10).The resulted aqueous phase was extracted again with chloroform (4x) to recover the monoacylated product. The organic phase with monoacylated product was washed with water (4x), dried over MgSO4 and concentrated to give (1) (0.809 g, 50% in two steps) asa colorless oil

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

Reference£º
Patent; CENTRE NATIONAL DE LA RECHERCHE SCIENTIFIQUE; UNIVERSITE D’ORLEANS; AGROFOGLIO, Luigi; ROY, Vincent; PLEBANEK, Elzbieta; BESSIERES, Maxime; (105 pag.)WO2018/50771; (2018); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics