Analyzing the synthesis route of 103-76-4

The synthetic route of 103-76-4 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.103-76-4,N-(2-Hydroxyethyl)piperazine,as a common compound, the synthetic route is as follows.

A mechanically-stirred solution of 1-(2-hydroxyethyl)piperazine (10.0 g, 9.4 mL, 0.07 mol) in 30 mL of deionized water is cooled to 0 C. Then portions of 4N sodium hydroxide (total 28 mL) and portions of benzyl chloroformate (18.8 g, 15.7 mL, 0.11 mol) are added over 15 minute periods, keeping the temperature at 0 C. to 5 C. At the end of the additions, 4N sodium hydroxide solution is added to bring the pH of the reaction mixture to 10. After 1 hour dichloromethane (200 mL) is added and the layers are separated. The organic solution is dried over anhydrous sodium sulfate and evaporated under reduced pressure to give 1-(2-hydroxyethyl)-4-carbobenzyloxypiperazine., 103-76-4

The synthetic route of 103-76-4 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Mallinckrodt Medical, Inc.; US5554749; (1996); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Analyzing the synthesis route of 103-76-4

As the paragraph descriping shows that 103-76-4 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.103-76-4,N-(2-Hydroxyethyl)piperazine,as a common compound, the synthetic route is as follows.

The preparation method of 4-hydroxyethylpiperazine ethanesulfonic acid includes the following steps: 1) Mix 260g (2mol) 2-hydroxyethylpiperazine, 165g (0.94mol) sodium 2-chloroethylsulfonate with 120mL water, stir well, the reaction solution becomes clear, the pH is about 10,Heat up to 85 , stop heating until the system self-heats to 103-105 ,The reaction is heated to reflux for 30min, the reaction is over, and the pH is about 8;2) Cool the reaction liquid to 60 C, add triethylamine to the reaction liquid to adjust the pH to 7-8, 1.5 L of absolute ethanol and 8 g of activated carbon, boil for 30 min, and filter while hot;3) Adjust the pH of the filtrate to 5 using glacial acetic acid, stir the filtrate and cool to 5 C to crystallize overnight,Filter and dry to obtain 310g of crude product, which is 95% by drying after titration inspection; 4) Dissolve the sample obtained in step 3) in 750 mL of ethanol and heat to reflux, Add 145mL of water, stir to dissolve, filter while hot, and the filtrate is cooled to 5 overnight, Filtration gave 181g of 4-hydroxyethylpiperazineethanesulfonic acid crystals, After drying, 175g of 4-hydroxyethylpiperazineethanesulfonic acid was obtained, and the content was 99.8% after titration; 5) Concentrate the mother liquor under reduced pressure to a volume of 30-40%, add activated carbon to boil for decolorization, filter while hot, the filtrate is cooled to 0-5 C, filtered, dried and recovered to obtain 15g of 4-hydroxyethylpiperazineethanesulfonic acid After titration, the content was 99.6%, and the total yield was 84.7%., 103-76-4

As the paragraph descriping shows that 103-76-4 is playing an increasingly important role.

Reference£º
Patent; Suzhou Yake Technology Co., Ltd.; Yuan Yongkun; (10 pag.)CN110683995; (2020); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Brief introduction of 103-76-4

103-76-4, The synthetic route of 103-76-4 has been constantly updated, and we look forward to future research findings.

103-76-4, N-(2-Hydroxyethyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

[0138]1-(2-hydroxyethyl)piperazine (Compound 3) (16.6 g, 127.6 mmol)) and 2-methyl-4,6-dichloropyrimidine (Compound 2) (10.4 g, 63.8 mmol) were mixed with methylene dichloride (80 mL) in reaction flask to be stirred for 2.5 h at 30 C., and then triethylamine (1.8 mL) was added with the reaction overnight in thermal insulation. After vacuum filtration, the cake was rinsed by methylene dichloride. The filtrate was vacuum condensed to dry, and then n-hexane (40 mL) was added to grow the grains for 1 h by stirring. After vacuum filtration, the cake was rinsed by n-hexane (20 mL) and dried at 40 C. to constant weight to give white solid target Compound 4 (14.7 g, yield: 89.8%).[0139]Element analysis: C11H17ClN4O, Calculated: C, 51.46; H, 6.67; N, 21.82. Found: C, 51.45; H, 6.69; N, 21.82.

103-76-4, The synthetic route of 103-76-4 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Nan Jing Cavendish Bio-Engineering Technology Co. Ltd.; Yan, Rong; Yang, Hao; Hou, Wen; Xu, Yongxiang; US2013/30177; (2013); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Downstream synthetic route of 103-76-4

As the paragraph descriping shows that 103-76-4 is playing an increasingly important role.

103-76-4, N-(2-Hydroxyethyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,103-76-4

In THF (30 ml) were added N-(2-hydroxyethyl)piperazine (500 mg, 3.84 mmol), a solution of formaldehyde (3117 mg, 38.41 mmol) and sodium cyanoborohydride (1207 mg, 19.20 mmol). The mixture was heated up to 50 C. overnight under stirring. After cooling some water was added and the mixture was extracted with DCM (3¡Á). The organic layers were dried over MgSO4 and evaporated. The residue was purified over a silica plug with DCM/MeOH 9:1 as eluant to afford an oil (370 mg, Y=67%). 1H NMR (DMSO-d6) delta 4.45 (t, J=5.3 Hz, 1H), 3.51-3.45 (m, 2H), 3.02-2.84 (m, 4H), 2.71-2.64 (m, 2H), 2.61 (s, 3H), 2.58-2.53 (m, 2H), 2.47-2.43 (m, 2H).

As the paragraph descriping shows that 103-76-4 is playing an increasingly important role.

Reference£º
Patent; ARES TRADING S.A.; US2008/51397; (2008); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Analyzing the synthesis route of 103-76-4

103-76-4, The synthetic route of 103-76-4 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.103-76-4,N-(2-Hydroxyethyl)piperazine,as a common compound, the synthetic route is as follows.

5mmol N,N-dimethylglycine,2mmol CuI,20mmol 4,6-dichloro-2-methylpyrimidine is soluble100 mL of N,N-dimethylformamide (DMF),22 mmol of N-hydroxyethylpiperazine was added with stirring.40mmol K3PO4, stir at room temperature for 40min,22 mmol of 2-amino-N-(2-chloro-6-methylphenyl)-5-thiazolecarboxamide was added with stirring.Passing N2 and reacting at 120 C for 6 h,The copper salt was dissolved in 50 mL of aqueous ammonia, and extracted with 50 mL of EtOAc (EtOAc).The crude product was added to 100 mL of an 80% aqueous ethanol solution, and stirred.2 g of activated carbon was added, refluxed for 30 min, filtered while hot, and the filtrate was recrystallized overnight, filtered, and the filter cake was washed with ice-cold 80% aqueous ethanol solution and dried.That is, 8.64 g of a white solid was obtained, the yield was 88.41%, and the purity was 99.92%.

103-76-4, The synthetic route of 103-76-4 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Shandong Luoxin Pharmaceutical Group Co., Ltd.; Shandong Luoxin Pharmaceutical Group Hengxin Pharmaceutical Co., Ltd.; Shandong Yuxin Pharmaceutical Co., Ltd.; Gao Hongjun; Ren Qingwei; Zhang Qingdong; (12 pag.)CN109879869; (2019); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Some tips on 103-76-4

103-76-4 N-(2-Hydroxyethyl)piperazine 7677, 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.103-76-4,N-(2-Hydroxyethyl)piperazine,as a common compound, the synthetic route is as follows.

103-76-4, [00212] Step 1 : To a solution of 4-fluoronitrobenzene (2.0g, 14.16 mmol) in AcN (15 mL), 2-(piperazin-l-yl)ethanol (1.85 g, 14.17mmol) and DIEA (2.97 mL, 17.01 mmol) were added. The mixture was refluxed for 15 h (in a sealed tube). After cooling, the resulting mixture was poured to water (300 ml). The mixture was stirred at room temperature for 30 min. The solids were collected by filtration and washed with water to afford the the desired product as off white solids (2.74g, 72% yield). ESI-MS calcd for (C12H17N303) 251, found 252 [M+H]+.

103-76-4 N-(2-Hydroxyethyl)piperazine 7677, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; NANTBIOSCIENCE, INC.; TAO, Chunlin; POLAT,, Tulay; WEINGARTEN, Paul; NALLAN, Laxman; ARP, Forrest; WANG, Qinwei; HO, David; (129 pag.)WO2016/138527; (2016); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Brief introduction of 103-76-4

103-76-4, The synthetic route of 103-76-4 has been constantly updated, and we look forward to future research findings.

103-76-4, N-(2-Hydroxyethyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: Substituted amine (1.2 equiv) was added to a mixture of 4-fluoronitrobenzene (1 equiv) and K2CO3 (2.0 equiv) in DMF (7mL/g). The reaction mixture was stirred at 40C and followed by TLC. After completion of the reaction, the mixture was poured into stirring ice-water. The resulting precipitate was filtered and dried to obtain compounds 11 as a yellow solid.

103-76-4, The synthetic route of 103-76-4 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Hou, Yunlei; Zhu, Liangyu; Li, Zhiwei; Shen, Qi; Xu, Qiaoling; Li, Wei; Liu, Yajing; Gong, Ping; European Journal of Medicinal Chemistry; vol. 163; (2019); p. 690 – 709;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Some tips on 103-76-4

103-76-4, 103-76-4 N-(2-Hydroxyethyl)piperazine 7677, 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.103-76-4,N-(2-Hydroxyethyl)piperazine,as a common compound, the synthetic route is as follows.

General procedure: 4,6-dichloro-2-methylpyrimidine 10a (1 mmol) and corresponding piperazine (2 mmol) were mixed in CH2Cl2 (40 mL) and stirred at room temparature overnight. The mixture was purified by flash chromatography (DCM: MeOH = 20:1) to give the product 1e-g.

103-76-4, 103-76-4 N-(2-Hydroxyethyl)piperazine 7677, apiperazines compound, is more and more widely used in various fields.

Reference£º
Article; Yan, Longjia; Deng, Minggao; Chen, Anchao; Li, Yongliang; Zhang, Wanzheng; Du, Zhi-yun; Dong, Chang-zhi; Meunier, Bernard; Chen, Huixiong; Tetrahedron Letters; vol. 60; 20; (2019); p. 1359 – 1362;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Some tips on 103-76-4

103-76-4, 103-76-4 N-(2-Hydroxyethyl)piperazine 7677, 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.103-76-4,N-(2-Hydroxyethyl)piperazine,as a common compound, the synthetic route is as follows.

General procedure: 4,6-dichloro-2-methylpyrimidine 10a (1 mmol) and corresponding piperazine (2 mmol) were mixed in CH2Cl2 (40 mL) and stirred at room temparature overnight. The mixture was purified by flash chromatography (DCM: MeOH = 20:1) to give the product 1e-g.

103-76-4, 103-76-4 N-(2-Hydroxyethyl)piperazine 7677, apiperazines compound, is more and more widely used in various fields.

Reference£º
Article; Yan, Longjia; Deng, Minggao; Chen, Anchao; Li, Yongliang; Zhang, Wanzheng; Du, Zhi-yun; Dong, Chang-zhi; Meunier, Bernard; Chen, Huixiong; Tetrahedron Letters; vol. 60; 20; (2019); p. 1359 – 1362;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Brief introduction of 103-76-4

103-76-4, The synthetic route of 103-76-4 has been constantly updated, and we look forward to future research findings.

103-76-4, N-(2-Hydroxyethyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: Substituted amine (1.2 equiv) was added to a mixture of 4-fluoronitrobenzene (1 equiv) and K2CO3 (2.0 equiv) in DMF (7mL/g). The reaction mixture was stirred at 40C and followed by TLC. After completion of the reaction, the mixture was poured into stirring ice-water. The resulting precipitate was filtered and dried to obtain compounds 11 as a yellow solid.

103-76-4, The synthetic route of 103-76-4 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Hou, Yunlei; Zhu, Liangyu; Li, Zhiwei; Shen, Qi; Xu, Qiaoling; Li, Wei; Liu, Yajing; Gong, Ping; European Journal of Medicinal Chemistry; vol. 163; (2019); p. 690 – 709;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics