Simple exploration of N-(2-Hydroxyethyl)piperazine

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

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

To a stirred solution of 1-(2-hydroxyethyl)piperazine (26 g, 0.2 mol) in DMF (200 mL) was added formic acid (752 mL, 0.2 mol) and formaldehyde (16.2 g, 0.2 mol, 37% solution in water). The reaction mixture was cautiously heated at 100 C. for 2 hours then stirred overnight at room temperature. The solvent was removed in vacuo. This procedure was repeated 3 further times to give 100 g of product. The crude products were combined and distilled under vacuum to give, at 74 C., 2-(4-methylpiperazin-1-yl)ethanol (51 g, 44%) as a colourless liquid.Analytical LCMS: (System B, RT=0.70 min), ES+: 145.1 [MH]+., 103-76-4

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

Reference:
Patent; Biovitrum AB; US2009/203695; (2009); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Simple exploration of N-(2-Hydroxyethyl)piperazine

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

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

a N-(tert-Butoxycarbonyl)-1-(2-hydroxyethyl)piperazine To a solution of 1-(2-hydroxyethyl)piperazine (5.20 g, 40 mmol) and triethylamine (6 mL) in 1,4-dioxane (100 mL) was added slowly di-tert-butyl dicarbonate (8.72 g, 40 mmol). The reaction mixture was stirred at room temperature for 2 h. The solvent was removed in vacuo and the residue was purified by flash column chromatography (ethyl acetate to 2% methanol in ethyl acetate) to give the title compound as a colorless oil (8.32 g, 90%). 1 H-NMR (300 MHz, CDCl3) delta 1.46 (s, 9H), 2.46 (t, 4H), 2.55 (t, 2H), 2.75 (bs, 1H), 3.44 (t, 4H), 3.63 (t, 2H)., 103-76-4

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

Reference:
Patent; 3-Dimensional Pharmaceuticals, Inc.; US5792769; (1998); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Simple exploration of N-(2-Hydroxyethyl)piperazine

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

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

To a stirred suspension of 1-fluoro-4-nitrobenzene (2 g,14.17 mmol) and potassium carbonate (3.92 g, 28.3 mmol) in anhydrous dimethyl sulfoxide (10 mL) was added 2- (piperazin-1-yl)ethanol (2.089 mL, 17.01 mmol) and the mixture was heated at 80 C for 16 hours. After coolingthe mixture was partitioned between water (100 mL) and ethyl acetate (30 mL) . The aqueous layer was separated and extracted with ethyl acetate (2 x 30 mL) . The combined organic fractions were reduced in vacuo. The residue was triturated in water (100 mL) . The solid wascollected by filtration under vacuum and dried for 16 hours under vacuum and flowing nitrogen to give the title compound (3.45 g, 97 %) . ?H NMR (400 MHz, CDC13) : 3 8.11 (d, 2H), 6.82 (d, 2H), 3.68 (t, 2H), 3.44 (t, 4H), 2.67 (t, 4H), 2.62 (t, 2H), 2.55 (br s, 1H) . LCMS (Method C):RT = 0.45 mi m/z = 252 [M+H]., 103-76-4

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

Reference:
Patent; ALMAC DISCOVERY LIMITED; HARRISON, Timothy; TREVITT, Graham; HEWITT, Peter Robin; O’DOWD, Colin Roderick; BURKAMP, Frank; WILKINSON, Andrew John; SHEPHERD, Steven D.; MIEL, Hugues; WO2015/92431; (2015); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Simple exploration of 103-76-4

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

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

A solution of 2-(piperazin-1-yl)ethan-1-ol (0.943 mL, 7.681 mmol) and di-tert-butyl dicarbonate (1.760 g, 8.065 mmol) in tetrahydrofuran (5 mL) was stirred at the room temperature for 18 hr. Then, water was added to the reaction mixture, followed by extraction with ethyl acetate. The organic layer was washed with aqueous saturated sodium chloride solution, dried with anhydrous MgSO4, filtered, and concentrated in vacuo. The residue was chromatographed (SiO2, 24 g cartridge; methanol / dichloromethane = 0 % to 10 %) to give tert-butyl 4-(2-hydroxyethyl)piperazine-1-carboxylate as colorless oil (1.750 g, 98.9 %)., 103-76-4

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

Reference:
Patent; CHONG KUN DANG PHARMACEUTICAL CORP.; LEE, Jaekwang; HAN, Younghue; KIM, Yuntae; MIN, Jaeki; BAE, Miseon; KIM, Dohoon; JIN, Seokmin; KYUNG, Jangbeen; (191 pag.)WO2017/18805; (2017); 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.

To a solution of 1-(2-hydroxyethyl)piperazine (51.7 g, 398 mmol) in DCM (500 mL) was added NEt3 (70.0 mL, 526 mmol) and di-tert-butyl dicarbonate (80.0 g, 367 mmol). The reaction mixture was stirred overnight at room temperature and then washed with 1M aq Na2CO3 solution (2×300 mL), dried (MgSO4) and concentrated in vacuo to give tert-butyl 4-(2-hydroxyethyl)piperazine-1-carboxylate (66.0 g, 72%) as a colourless oil.Analytical LCMS: (System B, RT=1.54 min), ES+: 231.4 [MH]+.

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

Reference:
Patent; Biovitrum AB; US2009/203695; (2009); A1;,
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.

The 5 mmol N, N – dimethyl glycine, 2 mmol CuI, 20 mmol 4, 6 – dichloro -2 – methyl pyrimidine dissolved in 100 ml DMF, under stirring, add 22 mmol N – hydroxyethyl piperazine, 40 mmol K3PO4, Stirring at room temperature for 40 min, added under mixing 2 – amino – N – (2 – chloro -6 – methyl phenyl) -5 – thiazole carboxamide 22 mmol. Through N2, For 120 C lower reaction 6 h after, adding 50 ml ammonia dissolved copper salt, for 50 ml × 3 ethyl acetate extraction, the combined acetic acid ethyl ester, saturated salt water for washing, the organic layer using anhydrous Na2SO4Drying, get the crude product. The crude product by adding 80% ethanol aqueous solution 100 ml, under stirring, by adding 2 g of activated carbon, reflux 30 min, is still hot filtration, filtrate refrigeration crystallization overnight, filtered, the filter cake of ice 80% ethanol aqueous solution washing, drying, to obtain white solid 8.64 g, yield 88.41% above, purity 99.92% above.

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

Reference:
Patent; Shandong Luoxin Pharmaceutical Group Co., Ltd.; Shandong Luoxin Pharmaceutical Group Hengxin Pharmaceutical Co., Ltd.; Shandong Yuxin Pharmaceutical Co., Ltd.; Gao Hongjun; Lv Peng; Yang Jianzhu; (11 pag.)CN109369638; (2019); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Analyzing the synthesis route of N-(2-Hydroxyethyl)piperazine

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.

1-[2-(tert-Butyl-diphenyl-silanyloxy)-ethyl]-piperazine To 2-piperazin-1-yl-ethanol (2 g, 15.36 mmol) in CH2Cl2 (70 mL) and pyridine (1.85 mL, 23.04 mmol) was added DMAP (188 mg, 1.53 mmol) and TBDPS chloride (3.37 mL, 18.44 mmol) and the reaction mixture stirred at RT for 18 h. The reaction mixture was concentrated in vacuo and the crude material was purified by silica gel column chromatography, eluting with CH2Cl2 and increasing the polarity to 10% MeOH/CH2Cl2 to obtain 1-[2-(tert-butyl-diphenyl-silanyloxy)-ethyl]-piperazine as a colourless oil (1.1 g, 21%). AnalpH2_MeOH-4 min(3): Rt 2.48 min; m/z 369 [M+1]+., 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; Ashworth, Alan; Lord, Christopher James; Elliot, Richard James Rowland; Niculescu-Duvaz, Dan; Porter, Roderick; Boffey, Raymond John; Bayford, Melanie Jayne; Firth-Clark, Stuart; Jarvis, Ashley Nicholas; Perrior, Trevor Robert; Key, Rebekah Elisabeth; US2015/99732; (2015); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Brief introduction of 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,103-76-4

(1) Preparation of 1-tert-butoxycarbonyl-4-(2-hydroxyethyl)piperazine To a solution of 10.00 g of 1-(2-hydroxyethyl)piperazine in 70 mL of dioxane at room temperature was added dropwise a solution of 16.43 g of di-tert-butyl dicarbonate in 30 mL of 1,4-dioxane with stirring. After completion of the reaction, the mixture was concentrated and n-hexane was added to the residue. The solid was collected by filtration and dried to give 14.11 g of the title compound.

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

Reference£º
Patent; Mitsui Chemicals, Inc.; US5969138; (1999); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Brief introduction of N-(2-Hydroxyethyl)piperazine

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

131.5 g of N-hydroxyethylpiperazine (purity 99%, about 1 mol)And 30% (mass concentration) aqueous sodium vinyl sulfonate solution (containing 1.05 mol of sodium vinyl sulfonate)Was added to a 1000 mL four-necked flask equipped with a reflux tube,The addition reaction is carried out with sufficient stirring;The reaction was carried out at 60 C for 1.0 hour,And then gradually heated to boiling reflux (about 100 ~ 120 , depending on the composition of the reaction and change)And continue to react for 2.0 hours;then,Cooled to give a reaction mother liquorcontaining 4-hydroxyethylpiperazineethanesulfonate.By high performance liquid chromatography,The yield of sodium 4-hydroxyethylpiperazineethanesulfonate was calculated to be 95.2%.A reaction mother liquor containing 0.5 mol HEPES-Na at a mass concentration of 40 wt% was placed in a 500 mL beaker,Under stirring,At room temperature,27.3 g of oxalic acid (99 wt%) was added slowly,Then stir,And acidified at 20 C for 1 hour.Into the low temperature thermostat,Cooling to 10 ,Cooling crystallization for 0.5 hours,The precipitated sodium oxalate was removed by filtration.The filtrate was placed in a beaker,Constantly stirring,1.0 g of Ba (OH) 2 was slowly added,Reaction for 1 hour,Remove the sulfate.Adding 5 g of activated carbon decolorization and filtering by filtration to obtain the filtrate,By rotary evaporation to anhydrous,To obtain a solid primary purified product.The solids were washed three times with 500 ml of ethanol,And then vacuum drying,Get high purity HEPES.

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

Reference£º
Patent; Shandong University of Technology; Cui Hongyou; Wang Jiangang; Zhu Liwei; Liu Ransheng; Yang Yong; Wang Yang; (8 pag.)CN104803949; (2017); B;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Downstream synthetic route of N-(2-Hydroxyethyl)piperazine

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

Compound 45A: tert-but l 4-(2-hydroxyethyl)piperazine-l-carboxylate 2-(piperazin-l-yl)ethan-l-ol (5 g, 38.41 mmol, 1.00 equiv) was dissolved in DCM (100 mL), and a solution of di-tert-butyl dicarbonate (8.38 g, 38.40 mmol, 1.00 equiv) in DCM (20 mL) was added drop-wise. The reaction was left under agitation overnight at ambient temperature. The reaction was evaporated to dryness and the residue dissolved in 200 mL of AcOEt, washed 5 times with NaCl (sat.), dried over sodium sulfate, filtered and concentrated under reduced pressure to yield 8.5 g (96 %) of compound 45 A in the form of a white solid.

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

Reference£º
Patent; PIERRE FABRE MEDICAMENT; RILATT, Ian; PEREZ, Michel; GOETSCH, Liliane; BROUSSAS, Matthieu; BEAU-LARVOR, Charlotte; HAEUW, Jean-Francois; WO2015/162293; (2015); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics