Month: November 2020

1214196-85-6, 1-(tert-Butoxycarbonyl)piperazine-2-carboxylic acid is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a solution of Compound ID (320 mg, 1.35 mmol) in EtOH (10 mL) was added l-(tert-butoxycarbonyl)piperazine-2-carboxylic acid (311 mg, 1.35 mmol), Nal (125 mg, 0.675 mmol), and Na2CCb (574 mg, 5.42 mmol). The mixture was stirred at 78 C for 15 hours and concentrated under reduced pressure. The resulting solid was dissolved in methanol and dichloromethane (50 ml, v/v 5/100), filtered, and concentrated to furnish Compound IE: LC-MS (ESI) m/z: 431 [M+H]+., 1214196-85-6

As the paragraph descriping shows that 1214196-85-6 is playing an increasingly important role.

Reference£º
Patent; BIOMARIN PHARMACEUTICAL INC.; WANG, Bing; (270 pag.)WO2019/104011; (2019); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

109-01-3, 1-Methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Add 10 g (46.3 mmol) of p-nitrobenzyl bromide and 100 mL of dichloromethane to a 500 mL single-necked flask. A mixture of 4.7 g (47.0 mmol) of N-methylpiperazine and 7.1 g (70.3 mmol) of triethylamine in 20 mL of dichloromethane was slowly added dropwise under ice-water bath (0-5 C). After heating and refluxing for 1 hr, the material disappeared by TLC (ethyl acetate: petroleum ether = 1:2). 150 mL of chloroform and 100 mL of a saturated sodium hydrogencarbonate solution were added to the reaction mixture, and stirred vigorously at room temperature for 30 min. The reaction mixture was extracted with chloroform (100 mL¡Á3), and the organic layers were combined and washed with water and saturated sodium chloride (100 mL¡Á1). Dry over anhydrous magnesium sulfate, filter, The solvent was evaporated under reduced pressure to give 8.5 g of pale yellow solid. The yield was 78.1%, and the product was directly fed to the next reaction without further purification., 109-01-3

As the paragraph descriping shows that 109-01-3 is playing an increasingly important role.

Reference£º
Patent; Shanghai Fuxing Pharmaceutical Industrial Co., Ltd.; Lu Shuai; Jin Qiaomei; Wang Yue; Chen Yadong; Lu Tao; (54 pag.)CN104592251; (2019); B;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

109-01-3, 1-Methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

t-BOC-Protected methylpiperizine was heated in the presence of l-fluoro-4- nitrobenzene under pressure in benzene to give 4-t-BOC-protected 1-methyl-1- (4- nitrophenyl) piperazinium salt. The piperazinium salt was heated in the presence of potassium [F] fluoride and Krytofix at 200C for 10 minutes. The oil was treated with aq. 3 M HC1 for 20 minutes to give [F-18]-1-methyl-1-(4-fluorophenyl) piperazinium chloride, 109-01-3

As the paragraph descriping shows that 109-01-3 is playing an increasingly important role.

Reference£º
Patent; THE GENERAL HOSPITAL CORPORATION; WO2005/82425; (2005); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

31166-44-6, 1-Cbz-Piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A mixture of 1-Cbz piperazine (1 g, 4.55 mmol),2-bromo-2-methylpropionamide (751 mg, 4.55 mmol),potassium carbonate (942 mg, 6.83 mmol) and acetonitrile (10 mE) was stirred at 80¡ã C. overnight. The reaction mixture was filtered, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel colunm chromatography to obtain 57-c (1.05 g, 76percent). EC-MS (ESI): mlz 306.3 (M+H)., 31166-44-6

The synthetic route of 31166-44-6 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; SHANGHAI YINGLI PHARMACEUTICAL CO., LTD; XU, Zusheng; (174 pag.)US2016/214994; (2016); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

548762-66-9, (2S,5R)-tert-Butyl 2,5-dimethylpiperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,548762-66-9

In a round bottom flask, 2-(chloro(4-fluorophenyl)methyl)-3-fluoropyridine (790 mg, 3.30 mmol) was dissolved in acetonitrile (16.5 mL). To this solution, potassium iodide (54.7 mg, 0.330 mmol), triethylamine (0.919 mL, 6.59 mmol) and tert-butyl (2S,5R)-2,5-dimethylpiperazine-1-carboxylate (706 mg, 3.30 mmol) were added sequentially. After heating at 75 C for 5 hours, TLC in 2:3 ethyl acetate/hexanes showed a trace of starting material and two new compounds of lower rf. LSMS was consistent with 2 major products each having the correct MW corresponding to the two separable diastereomers. The crude material was chromatographed on a 24 g silica gel column with 10-50 % ethyl acetate in hexanes to separate two major fractions labeled Isolate-1 and Isolate-02. LCMS showed that each fraction was consistent with a single diastereomer contaminated with a small amount of the other diastereomer. (1453) Intermediate 157: Isolate-1, First eluting fraction. Analytical LCMS conditions: Injection Vol= 1 mL, Start %B 0, Final %B 100, Gradient Time 2 Minutes, Flow Rate 1 mL/min, Wavelength 220 nm, Solvent Pair Acetonitrile/ Water/ TFA, Solvent A 10 % acetonitrile/ 90 % water/ 0.05% TFA, Solvent B 10 Water 90 % acetonitrile/ 0.05% TFA, Column Acquity BEH C1821. X 50 mm 1.7 mm, Oven Temp= 40 C. LCMS results; retention time 1.27 minutes, observed mass 418.5 (MH+). (1454) Intermediate 158: Isolate-2, Second eluting fraction. Analytical LCMS conditions: Injection Vol= 1 mL, Start %B 0, Final %B 100, Gradient Time 2 Minutes, Flow Rate 1 mL/min, Wavelength 220 nm, Solvent Pair acetonitrile/water/TFA, Solvent A 10 % acetonitrile/90 % water/0.05% TFA, Solvent B 10 Water 90 % acetonitrile/0.05% TFA, Column Acquity BEH C1821. X 50 mm 1.7 mm, Oven Temp= 40 C. LCMS results; retention time 1.31 minutes, observed mass 418.1 (MH+).

548762-66-9 (2S,5R)-tert-Butyl 2,5-dimethylpiperazine-1-carboxylate 11745988, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; BRISTOL-MYERS SQUIBB COMPANY; VELAPARTHI, Upender; CHUPAK, Louis S.; DARNE, Chetan Padmakar; DING, Min; GENTLES, Robert G.; HUANG, Yazhong; KAMBLE, Manjunatha Narayana Rao; MARTIN, Scott W.; MANNOORI, Raju; MCDONALD, Ivar M.; OLSON, Richard E.; RAHAMAN, Hasibur; JALAGAM, Prasada Rao; ROY, Saumya; TONUKUNURU, Gopikishan; VELAIAH, Sivasudar; WARRIER, Jayakumar Sankara; ZHENG, Xiaofan; TOKARSKI, John S.; DASGUPTA, Bireshwar; REDDY, Kotha Rathnakar; RAJA, Thiruvenkadam; (0 pag.)WO2020/6018; (2020); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

109-07-9, 2-Methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Preparation of Benzoylpiperazines XXXI, XXXII, XXXVIII, Commercially available benzoic acid (4.8 g, 40 mmol), pentafluorophenol (7.4 g, 40 mmol) and EDAC (7.6 g, 40 mmol) were combined in 60 ml of dry DMF. The mixture was stirred at room temperature for 2 hours. To this solution, 2-methylpiperazine (4.0 g, 40 mmol) in 30 ml of DMF was added slowly and the reaction mixture was stirred at room temperature for 12 hours. Evaporation of DMF gave a residue which was diluted with 400 ml of EtOAc and washed with water (2*100 nm). The organic phase was dried over anhydrous MgSO4 and concentrated in vacuo to provide a crude product, which was purified by column chromatography with EtOAc/MeOH (100:1) and then EtOAc/MeOH (10:1) to give 4.8 g of product XX in 60% yield., 109-07-9

109-07-9 2-Methylpiperazine 66057, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; Bristol-Myers Squibb Company; US6469006; (2002); B1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

5747-48-8, 11-(Piperazin-1-yl)dibenzo[b,f][1,4]thiazepine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

In 5 mL of acetonitrile was dissolved 500 mg (1.693 mmol) of 11-piperazin-l- yldibenzo[b,fj[l,4]thiazepine. In 5 mL of acetonitrile at room temperature was dissolved 166 mg (1.693 mmol) H2SO4. The solutions were combined resulting in immediate precipitation of a gummy solid. The solid did not redissolve upon reheating, but did triturate into a free-flowing solid. The solids collapsed overnight into a gummy mass which was redissolved in methanol (50 mL) and stripped down to a granular solid which was triturated under acetone (20 mL), filtered, and dried under vacuum at 40 0C resulting in 660 mg (99%). mp 100-105 0C (sharp). 1H NMR (DMSO-dbeta) was consistent with the title salt.Polarized light microscopy revealed the material to be composed of agglomerates of very small crystalline particles. DSC revealed two large and three small endothermic events (Figure 7). Of the two large events, the lower temperature event may correspond to water/solvent loss and the higher temperature event may correspond to melt/decomposition. The three small events may correspond to form changes. DVS revealed that the material is hygroscopic with isotherms characteristic of a weak multi-hydrate (Figure 8). The experiment was terminated near the end of sorption phase of the second cycle. Data from the first cycle indicated that moisture was lost during the desorption phase that had not been lost during the initial drying phase. Approximately 2.5 mole equivalents of water were gained in the first cycle while nearly 4 mole equivalents were gained during the second cycle., 5747-48-8

Big data shows that 5747-48-8 is playing an increasingly important role.

Reference£º
Patent; ASTRAZENECA AB; WO2007/62336; (2007); A2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

694499-26-8, 4-((4-Methylpiperazin-1-yl)methyl)-3-(trifluoromethyl)aniline is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

694499-26-8, General procedure: Step 3: General protocol for the preparation of 5-{3-(phenylcarbamoyl)-benzylamino}-lH- pyrrolo[2,3-b]pyridine-2-carboxylic acid methyl ester 5-amino-iH-pyrrolo[2,3-b]pyridine-2-carboxylic acid methyl ester (1 eq) and 3-formyl- benzamide compound (1.1 eq) were stirred in a mixture of MeOH/AcOH (10/1; 0.06M) for 2h. Then NaBH3CN (1.2eq) was slowly added and the mixture was stirred under argon at RT overnight. The reaction was quenched by addition of saturated NaHC03 solution until neutrality. MeOH and acetic acid were evaporated. The crude was filtered and washed with water and Et20 before being purified on reverse phase (H20 l%TFA/MeCN 1%TFA 100/0, 0/100). MeCN was evaporated. The product was suspended in H20 and basified with saturated NaHC03 solution until pH = 8-9. The aqueous layer was extracted three times with AcOEt. The organic layer was dried over Na2S04, filtered and concentrated to give the expected product.

As the paragraph descriping shows that 694499-26-8 is playing an increasingly important role.

Reference£º
Patent; ORIBASE PHARMA; CHEVE, Gwenael; DAYDE-CAZALS, Benedicte; FAUVEL, Benedicte; BORIES, Cedric; YASRI, Abdelaziz; WO2014/102378; (2014); A1;,
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.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

150407-69-5, (S)-1-((Benzyloxy)carbonyl)-4-(tert-butoxycarbonyl)piperazine-2-carboxylic acid is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,150407-69-5

Step 2: 1 -Benzyl 4-fert-butyl 2-methyl (2,SV1.2.4-piperazinetricarboxylate (AA2); A solution of TMS-diazomethane (2.0 M in Et2O, 4.0 eq.) was added to a stirred 0.16 M solution of AAl in a toluene-MeOH mixture (2:1). The reaction mixture was stirred overnight at RT. Solvents were removed under reduced pressure. The residue was purified by column chromatography on silica gel, eluting with 20 to 100% EtO Ac/petroleum ether to give the title compound in 92 % yield. 97% ee by SFC. [CC]D20 -10.6 (c 1.00, CHCl3). 1H NMR (300 MHz, CDCl3, 300K) delta 7.37 (5H, m), 5.18 (2H, m), 4.79-4.57 (2H, m), 4.10-3.90 (2H, m), 3.75 (1.5H, s), 3.70 (1.5H, s), 3.34-3.30 (IH, m), 3.10 (IH, dd, J = 13.6, 4.4 Hz), 2.86 (IH, m), 1.45 (9H, s). MS (ES+) Ci9H26N2O6 requires 378, found: 401 (M+Na)+.

150407-69-5 (S)-1-((Benzyloxy)carbonyl)-4-(tert-butoxycarbonyl)piperazine-2-carboxylic acid 1512536, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; ISTITUTO DI RICERCHE DI BIOLOGIA MOLECOLARE P. ANGELETTI S.P.A.; BRANCA, Danila; FERRIGNO, Federica; HERNANDO, Jose, Ignacio, Martin; JONES, Philip; KINZEL, Olaf; MALANCONA, Savina; MURAGLIA, Ester; PALUMBI, Maria, Cecilia; PESCATORE, Giovanna; SCARPELLI, Rita; WO2010/23480; (2010); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics