Month: October 2020

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.129799-08-2,1-tert-Butyl 3-methyl piperazine-1,3-dicarboxylate,as a common compound, the synthetic route is as follows.

To a 50 mL of sealing tube were added 1-tert-butyl 3-methyl piperazine-1,3-dicarboxylate (500 mg, 2.05 mmol) , iodomethane (580mg, 4.10 mmol) , potassium carbonate (424 mg, 3.07 mmol) and acetone (10 mL) .The mixture was stirred at 50 for 6 h and concentrated. The residue was diluted withwater (20 mL) . The resulting mixture was extracted with DCM (10 mL ¡Á 3) . The combined organic layers were dried over anhydrous Na2SO4and concentrated to give 1-tert-butyl 3-methyl 4-methylpiperazine-1,3-dicarboxylate as a light yellow solid (290 mg, 54) . 1H NMR (400 MHz, CDCl3): delta ppm 4.65-4.83 (m, 1H) , 4.29-4.33 (m, 1H) , 4.18-4.23 (m, 1H) , 4.05-4.11(m, 1H) , 3.80-3.94 (m, 3H) , 3.88 (s, 3H) , 3.66 (s, 3H) , 1.48 (s, 9H) and MS-ESI: m/z 259.30 [M+H] +.

129799-08-2, As the paragraph descriping shows that 129799-08-2 is playing an increasingly important role.

Reference£º
Patent; SUNSHINE LAKE PHARMA CO., LTD.; ZHANG, Yingjun; LIU, Bing; YU, Tianzhu; ZHANG, Xiangyu; ZHANG, Shiguo; ZHANG, Jiancun; CHENG, Changchung; (426 pag.)WO2016/34134; (2016); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

59878-57-8, 1-(Cyclopropylcarbonyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

59878-57-8, The active amide intermediate prepared in step 1 was dissolved in 10 ml of methylene chloride,The solution was cooled to 0 to 10 C and then added dropwise to a solution of 1-cyclopropylcarbamoylpiperazine (2.62 g, 17 mmol) and triethylamine (7.1 ml, 51 mmol) in 20 ml of dichloromethane for 1.5 hours at 0 to 10 C , Washed with 30 ml of water 3 times, the organic layer concentrated dry, add ethanol – water mixture (1: 2, v / v) 50 ml,And the filtrate was stirred at 0-5 C for 10 hours. The filtrate was filtered and dried to obtain 6.8 g of orapani. The yield was 92.0% and the purity was 99.87%.

The synthetic route of 59878-57-8 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Shanghai Jin – yin Biological Technology Co., Ltd; Yang, Yinghua; Ji, Ye; Chen, Fangfang; Dai, Yi; (10 pag.)CN105503739; (2016); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

548762-66-9,With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.548762-66-9,(2S,5R)-tert-Butyl 2,5-dimethylpiperazine-1-carboxylate,as a common compound, the synthetic route is as follows.

To a solution of 4,4′-(chloromethylene)bis(fluorobenzene) (3.76 g, 15.75 mmol) in acetonitrile (15 mL) was added tert-butyl (2S,5R)-2,5-dimethylpiperazine-1-carboxylate (2.25 g, 10.50 mmol), followed by DIPEA (5.50 mL, 31.5 mmol). The reaction mixture was stirred at 85 C overnight. The reaction mixture was concentrated under reduced pressure to remove volatiles, the residue was dissolved in ethyl acetate (150 mL), and washed with water. The aqueous layer was back-extracted with ethyl acetate (100 mL x 2). The combined organic layer was washed with brine, dried over Na2SO4 and concentrated under reduced pressure to give the crude product, which was purified by silica gel chromatography on ISCO (5-10 % EtOAc/petroleum ether; 80 g column) to afford tert-butyl (2S,5R)-4-(bis(4-fluorophenyl)methyl)-2,5-dimethylpiperazine-1- carboxylate (3.55 g, 81 % yield). LCMS: m/z = 417.4 (M+H); rt 1.561 min. (LCMS Condition: Column: Kinetex XB-C18 (3 x 75 mm) 2.6 mm; Mobile phase A: 10 mM ammonium formate:acetonitrile (98:2), Mobile phase B: 10 mM ammonium (0508) formate:acetonitrile (2:98), Gradient = 20-100 % B over 4 minutes, then a 0.6 minute hold at 100 % B; Temperature: 27 C; Flow rate: 1.0 mL/min; Detection: UV at 220 nm).

As the paragraph descriping shows that 548762-66-9 is playing an increasingly important role.

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

16154-72-6, 3-Chloro-4-(4-methylpiperazin-1-yl)benzenamine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To obtain the title compound of Example 31 , 5-(2-chloro-4-pyrimidinyl)-lambda/-ethyl-4-[3- methyl-5-(methyloxy)phenyl]-1 ,3-thiazol-2-amine (0.066 g, 0.183 mmol), prepared by a procedure analogous to Example 25, Step F, and [3-chloro-4-(4-methyl-1- piperazinyl)phenyl]amine (0.041 g, 0.183 mmol) were combined with iPrOH (2 ml.) and concentrated HCI (2 drops) in a microwave vial. The reaction was heated to 18O0C for 20 min in the microwave then cooled to rt. TEA (approx. 0.1 ml.) and silica gel were combined with the reaction and the resulting mixture was concentrated to dryness and subsequently adhered to silica gel. Column chromatography using EtOAc, MeOH, and NH4OH yielded fractions which were concentrated to dryness. This material was then further purified on a reverse phase acidic HPLC. The resulting fractions were free-based via extraction and concentrated to dryness to yield 35 mg of the title compound of Example 31 (35%Y). 1H NMR (400 MHz,DMSO-d6) delta 9.51 (s, 1 H), 8.25 (t, J = 5.4 Hz, 1 H), 8.07 (d, J = 5.6 Hz, 1 H), 8.03 (d, J = 2.5 Hz, 1 H), 7.54 (dd, J = 8.8, 2.6 Hz, 1 H), 7.06 (d, J = 8.9 Hz, 1 H), 6.88 (s, 1 H), 6.82 (d, J = 9.7 Hz, 2 H), 6.29 (d, J = 5.5 Hz, 1 H), 3.72 (s, 3 H), 3.28 (m, 2 H), 2.91 (br, 4 H), 2.48 (m, 4 H), 2.30 (s, 3 H), 2.23 (s, 3 H), 1.19 (t, J = 7.0 Hz, 3 H). HRMS C28H33N7OSCI (M+H)+ calcd 550.2156, found 550.2167.

16154-72-6, The synthetic route of 16154-72-6 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; SMITHKLINE BEECHAM CORPORATION; WO2009/32667; (2009); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

208167-83-3, tert-Butyl 4-(2-chloroethyl)piperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Preparation of tert-butyl 4-(2-((3-cyano-4-(6-(4-(5-fluoro-2- methylbenzamido)-4-methylpiperidin-l-yl)pyridin-3-yl)pyrazolo[l,5-a]pyridin-6- yl)oxy)ethyl)piperazine-l-carboxylate. To a mixture of N-(l-(5-(3-cyano-6- hydroxypyrazolo[l,5-a]pyridin-4-yl)pyridin-2-yl)-4-methylpiperidin-4-yl)-5-fluoro-2- methylbenzamide (Intermediate P68; 55 mg, 0.114 mmol), tert-Butyl 4-(2- chloroethyl)tetrahydro-l(2H)-pyrazine carboxylate (57 mg, 0.227 mmol) was added cesium carbonate (148 mg, 0.454 mmol) in DMA (1 mL) and was stirred overnight at 60C. After cooling to ambient temperature, reaction was diluted with EtOAc and washed with water and the organic extracts were dried over anhydrous Na2S04(S), filtered and concentrated in vacuo. The residue was purified using silica chromatography (50-100%) EtOAc in Hexanes) to afford the title compound (49 mg, 62% yield) MS (apci) m/z=697.4 (M+H).

208167-83-3, 208167-83-3 tert-Butyl 4-(2-chloroethyl)piperazine-1-carboxylate 22106269, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; ANDREWS, Steven W.; ARONOW, Sean; BLAKE, James F.; BRANDHUBER, Barbara J.; COLLIER, James; COOK, Adam; HAAS, Julia; JIANG, Yutong; KOLAKOWSKI, Gabrielle R.; MCFADDIN, Elizabeth A.; MCKENNEY, Megan L.; MCNULTY, Oren T.; METCALF, Andrew T.; MORENO, David A.; RAMANN, Ginelle A.; TANG, Tony P.; REN, Li; WALLS, Shane M.; (946 pag.)WO2018/71454; (2018); A1;,
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

5747-48-8, Preparation BA toluene solution of 1 l-piperazin-l-yldibenzo[b,fj[l,4]thiazepine (1500 mL, 0.686 mol) prepared by reaction of piperazine with 1 l-chloro-dibenzo[b,fj[l,4]-thiazepine in toluene (see, e.g., U. S. Pat. No. 4,879,288) was treated with 1500 mL deionized water and 90 mL of HCl (32% w/w). The resulting mixture was heated to 70 0C and agitated for 45 min. Agitation was ceased and the mixture allowed to settle and phase separate for 30 min. The lower aqueous phase, containing the HCl salt of 1 l-piperazin-l-yldibenzo[b,fj[l54]thiazepine was isolated. The aqueous phase was then treated with 1000 mL of toluene and 99 g of aqueous NaOH (47% w/w). The resulting mixture was heated to 70 C and agitated for 45 EPO min. Agitation was ceased and the mixture allowed to settle and phase separate for 30 min. The lower aqueous phase was discarded and the upper organic phase retained to which 300 mL of deionized water was added. The resulting mixture was agitated for 15 min and then allowed to settle for 30 min. The aqueous phase was discarded and the organic phase retained. The organic phase was extracted once more with 300 mL of deionized water. About 750 mL of toluene from the organic phase was distilled out. The resulting concentrate was cooled to 60 C, then 200 mL of methyl-t-butyl ether (MTBE) was added. The resulting mixture was cooled to ambient temperature then seeded with Form A seed crystals. The seeded mixture was then cooled to 10 C and held at this temperature for 3 hours under slow agitation. The resulting solid was isolated under suction via a no. 3 sinter. The solid product was then washed with 120 mL of MTBE at ambient temperature and dried at 40 C under vacuum resulting in 175 g (86.4%) of crystalline product. Assay 99.9% w/w by HPLC area %.

The synthetic route of 5747-48-8 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; ASTRAZENECA AB; WO2006/73360; (2006); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

129779-30-2, (3R,5S)-rel-tert-Butyl 3,5-dimethylpiperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

The (2i?,65)-l-(iV-benzyloxycarbonylglycyl)-2,6-dimethylpiperazine used as a starting material was prepared as follows :-; Diisopropylethylamine (0.4 ml) was added to a stirred mixture of ter t-butyl (3i?,55)-3,5-dimethylpiperazine-l-carboxylate (0.25 g; available from Atlantic SciTech Group, Inc., 601 East Linden Avenue, Linden, New Jersey 07036, USA)), N- benzyloxycarbonylglycine (0.296 g), 2-(7-azabenzotriazol-l-yl)-l,l,3,3-tetramethyluronium hexafluorophosphate (V) (0.555 g) and DMA (15 ml) and the resultant mixture was stirred at ambient temperature for 18 hours. The reaction mixture was evaporated and the residue was dissolved in a mixture of trifluoroacetic acid (1.5 ml) and methylene chloride (4.5 ml). The mixture was stirred at ambient temperature for 1 hour. The resultant mixture was evaporated. Methanol was added to the residue and the solution was loaded onto an Isolute SCX-2 cation exchange cartridge (20 g). The column was washed with methanol and the product was eluted using a 3M methanolic ammonia solution. There was thus obtained (2i?,6.S)-l-(N-benzyloxycarbonylglycyl)-2,6-dimethylpiperazine (0.46 g); Mass Spectrum: M+H+ 306; HPLC: method Bl, Retention Time 2.37 minutes.

129779-30-2, As the paragraph descriping shows that 129779-30-2 is playing an increasingly important role.

Reference£º
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2008/32064; (2008); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

208167-83-3, tert-Butyl 4-(2-chloroethyl)piperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Intermediate 117(R)-ethyl 1-((1-(2-(4-(tert-butoxycarbonyl)piperazin-1-yl)ethyl)pyrrolidin-3-yl)methyl)-6-(6-(3-ethylureido)-4-(4-(trifluoromethyl)thiazol-2-yl)pyridin-3-yl)-4-oxo-1,4-dihydroquinoline-3-carboxylateTo a vial was charged (R)-ethyl 6-(6-(3-ethylureido)-4-(4-(trifluoromethyl)thiazol-2-yl)pyridin-3-yl)-4-oxo-1-(pyrrolidin-3-ylmethyl)-1,4-dihydroquinoline-3-carboxylate (Intermediate 115) (50 mg, 0.081 mmol), tert-butyl 4-(2-chloroethyl)piperazine-1-carboxylate (23 mg, 0.090 mmol) and potassium carbonate (15 mg, 0.11 mmol) in anhydrous acetonitrile (2 mL) and the resulting mixture was stirred at 60-65 C. for 1.5 hours. The mixture was then diluted with saturated sodium bicarbonate and the product extracted with ethyl acetate. The organics were dried over sodium sulfate, concentrated, and purified with another lot (1.3 mmol) by Analogix eluting with dichloromethane/methanol.MS (ESP): 827.1 (MH+) for C40H49F3N8O6S, 208167-83-3

As the paragraph descriping shows that 208167-83-3 is playing an increasingly important role.

Reference£º
Patent; ASTRAZENECA AB; US2010/317624; (2010); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

109384-27-2, 1-Methylpiperazin-2-one hydrochloride is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

109384-27-2, To a mixture of 6-chloro-3-nitro-2-picoline (500 mg, 2.84 mmol) and 1-methyl-piperazin-2-one hydrochloride (535 mg, 3.55 mmol) in dioxane (15 ml) were added Cs2CO3 (1215 mg, 3.69 mmol) and xantphos (25.4 mg, 0.043 mmol). The mixture was degassed with Argon for 5 min, then Pd(OAc)2 (6.37 mg, 0.028 mmol) was added. The light brown suspension was heated up to 1 100C and stirred for 18h. The reaction mixture was concentrated then diluted in EtOAc/NaHCO3 aq. sat. soP. The aqueous layer was extracted twice with EtOAc. The combined organics were washed with brine, dried (Na2SO4) and after filtration, the solvent was removed under reduced pressure and the crude product was dried under high vacuum (500C). Purification was done by chromatography on silica gel (eluting with DCM / MeOH; 99/1 then 98/2) to obtain the title compound as a pink solid (347mg). (HPLC: tR 5.319 min (Method B); M+H = 251.2 MS-ES)

109384-27-2 1-Methylpiperazin-2-one hydrochloride 17060766, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; NOVARTIS AG; FURET, Pascal; IMBACH, Patricia; MAH, Robert; STAUFFER, Frederic; WO2010/139747; (2010); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

278788-66-2, (R)-tert-Butyl 3-(hydroxymethyl)piperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Step A: tert-butyl (3R)-4- [2-(3-cyano-4-fluoro-2-methylphenyll)-2-hydroxylethyli -3-(hydroxymethyl)piperazine- 1 -carboxylate: 6-Fluoro-2-methyl-3- (2-oxiranyl) benzonitrile(prepared as described above, 4.80 g, 27.1 rnmol) and (R)-4-N-BOC-2-hydroxymethyl-piperazine (8.79g. 40.6 rnmol) were suspended in EtOH (3OmL) and heated in a microwaveapparatus at 150 C for 1 h. The reaction mixture was cooled and evaporated to dryness. Theresidue was purified by chromatography through a 330 g ISCO Redi-sep column eluting with ethyl acetate to 5% MeOH/ ethyl acetate to yield the title compound. LC-MS: M+1= 394;

278788-66-2, As the paragraph descriping shows that 278788-66-2 is playing an increasingly important role.

Reference£º
Patent; MERCK SHARP & DOHME CORP.; PASTERNAK, Alexander; DEJESUS, Reynalda, Keh; FRIE, Jessica, L.; PIO, Barbara; TANG, Haifeng; WALSH, Shawn, P.; WO2014/99633; (2014); A2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics