Month: January 2021

181955-79-3, 1,4-Di-Boc-piperazine-2-carboxylic acid is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a dry flask were added 1, 4-di (tert-butoxycarbonyl) piperazine-2-carboxylic acid (14 g, 42.37 mmol) , potassium carbonate (11.7 g, 84.7 mmol) , acetone (200 mL) , iodomethane (5.3 mL, 85 mmol) in turn, the mixture was stirred at rt for 12 hours. The mixture was filtered, the filtrate was concentrated in vacuo and to the residue was added (200 mL) and water (200 mL) , the mixture was separated into layers, the organic layer was washed with saturated aqueous NaCl and dried over anhydrous sodium sulfate, then concentrated in vacuo to get the title compound as a white solid (13.55 g, 93%) . MS (ESI, pos. ion) m/z: 367.2 [M+Na] +.

181955-79-3, As the paragraph descriping shows that 181955-79-3 is playing an increasingly important role.

Reference£º
Patent; SUNSHINE LAKE PHARMA CO., LTD.; LIU, Xinchang; REN, Qingyun; YAN, Guanghua; GOLDMANN, Siegfried; ZHANG, Yingjun; (253 pag.)WO2019/76310; (2019); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

5625-67-2,With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.5625-67-2,Piperazin-2-one,as a common compound, the synthetic route is as follows.

To a solution of piperazinone (10.0 g, 100 mmol), Triethylamine (20.2 g, 200mmol), and DMAP (50 mg) in CHaCIa (250 ml) in an ice water bath was added(Boc)2O (22.9 g, 105 mmol) slowly. The mixture was stirred in the ice-water bath for 1h and at RT for 4.5 h. The mixture was diluted with CH2CI2 (250 ml), washed withwater (200 ml), 5% citric acid (200 ml), 1N HCI (200 ml), saturated sodiumbicarbonate (20 ml) and brine. The organic layer was dried (MgSO4) andconcentrated to give the product (18.0 g, 90%). MS m/e 201 (M+H)”1″

As the paragraph descriping shows that 5625-67-2 is playing an increasingly important role.

Reference£º
Patent; SCHERING CORPORATION; WO2006/14944; (2006); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

2762-32-5, Piperazine-2-carboxylic acid is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

54a. 4-((Benzyloxy)carbonyl)-1 -(tert-butoxycarbonyl)piperazine-2- carboxylic acidThe tile compound was prepared according to the procedure of [Kempf, D. J.; Norbeck, D. W.; Sham, H. L U.S. Patent 5,455,351 , Oct 3, 1995]. Piperazine-2-carboxylic acid (10.0 g, 77.0 mmol) was dissolved in a 1 :1 solution of 1 ,4-dioxane:water (100 mL) at room temperature with vigorous stirring. The clear solution was adjusted to pH 11 by the addition of an aqueous solution of sodium hydroxide (80 mL of a 1Lambda/ solution). The pH was monitored in situ with a pH meter throughout the reaction. The reaction flask was fitted with an addition funnel that contained a solution of Lambda/-alpha- (benzyloxycarbonyloxy) succinamide (13.6 g, 55 mmol) in 1 ,4-dioxane (50 mL). The Lambda/-alpha-(benzyloxycarbonyloxy) succinamide solution was added over 45 minutes at room temperature and the pH was kept above 10 by the periodic addition of 1 Lambda/ sodium hydroxide. The pH of the solution was adjusted to 9.5 and 2-(teAf-butoxycarbonyloxyimino)-2-phenylacetonitrile (13.4 g, 55 mmol) was added as a solution in 1 ,4-dioxane (50 mL) over 10 minutes. The pH was maintained at 9.5 and the solution was stirred at room temperature for 17 hours. The solution was then acidified to pH 2 and the aqueous solution was washed with diethyl ether (3 x 150 mL). The aqueous solution was cooled to O0C and acidified by adding of concentrated hydrochloric acid. The acidic solution was extracted with ethyl acetate (5 x 150 mL). The combined organic phases were dried over sodium sulfate, filtered and concentrated in vacuo. The residue was triturated with a 1 :1 solution of dichloromethane: hexanes (150 mL) and the solvent was removed in vacuo to provide the product as a viscous yellow oil (15.7 g, 43 mmol, 80%). Rf = 0.60 (66:34 dichloromethane: ethyl acetate + 0.1% (v/v acetic acid); 1H-NMR (400 MHz, DMSO) delta 13.0 (br s, 1 H), 7.37-7.36 (m, 5H), 5.05 (s, 2H), 4.54-4.33 (m, 2H), 3.90-3.66 (m, 2H), 3.07-2.81 (m, 4H), 1.38 (s, 9H); Mass spectrum (ESI +ve) m/z 365.1 (MH+).

2762-32-5, The synthetic route of 2762-32-5 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; BIKAM PHARMACEUTICALS, INC.; GARVEY, David, S.; LAROSA, Gregory, J.; GREENWOOD, Jeremy, Robert; BREWER, Mark, L.; QUACH, Tan; COTE, Jamie, B.; BERMAN, Judd; WO2010/147653; (2010); 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.5317-33-9,3-(4-Methylpiperazin-1-yl)propan-1-ol,as a common compound, the synthetic route is as follows.,5317-33-9

g) is thereby obtained in the form of cream-coloured crystals, m.p. 240 C. N-[3-(4-Methyl-1-piperazinyl)propoxy]phthalimide may be obtained in the following manner: a solution of 1-(3-hydroxypropyl)-4-methylpiperazine (8.4 g), N-hydroxyphthalimide (8.2 g) and triphenylphosphine (13.1 g) in tetrahydrofuran (120 cc) is cooled to a temperature in the region of 0 C. and ethyl azodicarboxylate (10.1 g) is added in the course of 30 minutes. The solution obtained is stirred at a temperature in the region of 20 C. for 18 hours and is then concentrated to dryness under reduced pressure (20 mm Hg; 2.7 kPa) at a temperature in the region of 60 C. The crude oil obtained is chromatographed on a column 5 cm in diameter containing silica (0.063-0.2 mm) (400 g). The column is eluted with mixtures of ethyl acetate and methanol, collecting 500-cc fractions. The first 5 fractions originating from elution with pure ethyl acetate and the next 5 fractions originating from elution with a mixture of ethyl acetate and methanol (70:30 by volume) are discarded. The next fraction originating from elution with a mixture of ethyl acetate and methanol (70:30 by volume), the next 5 fractions originating from elution with a mixture of ethyl acetate and methanol (50:50 by volume) and the next 2 fractions originating from elution with pure methanol are combined and concentrated to dryness under reduced pressure (20 mm Hg; 2.7 kPa) at a temperature in the region of 60 C. N-[3-(4-Methyl-1-piperazinyl)propoxy]phthalimide (11.4 g) is thereby obtained in the form of a red oil (Rf=0.2; thin-layer chromatography on silica, eluent: ethyl acetate/methanol, 50:50 by volume).

As the paragraph descriping shows that 5317-33-9 is playing an increasingly important role.

Reference£º
Patent; Rhone-Poulenc Sante; US5086051; (1992); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

216144-45-5, 4-(4-Methylpiperazin-1-yl)benzylamine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Preparation F; (3-chloro-4-(4-methylpiperazin-1-yl)phenyl)methanamine; Step F (1); To a solution of (4-(4-methylpiperazin-1-yl)phenyl)methanamine (204 mg, 1.0 mmol, Aldrich) in THF (2.0 mL) was added (Boc)2O (327 mg, 1.5 mmol) and NaOH/H2O (1.0 mL, 1 N). The mixture was stirred at rt for 1 h. EtOAc (100 mL) was added and the resulting solution was washed with H2O (2¡Á100 mL). The organic layer was dried and concentrated to give 250 mg (yield 82%) of tert-butyl 4-(4-methylpiperazin-1-yl)benzylcarbamate. LC-MS (M+H)+=306.35 1H-NMR(500 MHz, CD3OD) delta 7.18 (d, J=8.55 Hz, 2H), 6.94 (d, J=8.54 Hz, 2H), 4.15 (s, 2H), 3.16-3.22 (m, 4H), 2.60-2.66 (m, 4H), 2.36 (s, 3H), 1.46 (s, 9H).

216144-45-5, The synthetic route of 216144-45-5 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Bristol-Myers Squibb Company; US2007/49589; (2007); 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.74879-18-8,(S)-(+)-2-Methylpiperazine,as a common compound, the synthetic route is as follows.,74879-18-8

Step l; 3-(5)-Methyl-l-(5-trifluoromethyl-pyridin-2-yl)-piperazine:; 2-Bromo-5-trifluoromethyl-pyridine (1.06 g, 4.69 mmol), (5)-2-methylpiperazine (1.03 g, 10.28 mmol) and triethylamine (1.5 mL, 10.76 mmol) were stirred in toluene (10 mL) at 110 0C for 26 h. The reaction was cooled to room temperature, diluted with ethyl acetate (150 mL) and washed with water and brine. The organic layer was dried (MgSC>4), filtered and concentrated. The crude mixture was purified by automated silica gel flash column chromatography (gradient eluent 0-20% MeOH/dichloromethane) to afford 3-(S)-methyl-l-(5-trifluoromethyI-pyridin-2-yl)- piperazine (926 mg, 81 %) as a yellow solid. 1H NMR (400 MHz, CDCl3) delta 8.38 (s, IH), 7.62 (dd, IH), 7.63 (d, IH), 4.29-4.20 (m, 2H), 3.16-3.12 (m, IH), 3.02-2.85 (m, 3H), 2.64-2.52 (m, 2H), 1.18 (d, 3H).

As the paragraph descriping shows that 74879-18-8 is playing an increasingly important role.

Reference£º
Patent; KALYSPSYS, INC.; NOBLE, Stewart A.; OSHIRO, Guy; MALECHA, James W.; ZHAO, Cunxiang; ROBINSON, Carmen K. M.; DURON, Sergio G.; SERTIC, Michael; LINDSTROM, Andrew; SHIAU, Andrew; BAYNE, Christopher; KAHRAMAN, Mehmet; LOU, Boliang; GOVEK, Steven; WO2006/55187; (2006); A1;,
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Piperazines – an overview | ScienceDirect Topics

77279-24-4,77279-24-4, tert-Butyl 4-(2-hydroxyethyl)piperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Into a 50-mL round-bottom flask, was placed a solution of tert-butyl 4-(2-hydroxyethyl)piperazine-1-carboxylate (2.31 g, 10.03 mmol, 1.00 equiv) in dichloromethane (20 mL) and a solution of thionyl chloride (1.5 mL, 2.00 equiv) in dichloromethane (3 mL) was added dropwise at 0 C. The resulting solution was stirred overnight at 25 C. The resulting mixture was concentrated under vacuum. The resulting solution was diluted with 10 mL of water. The resulting solution was extracted with 2*25 mL of ethyl acetate and the organic layers combined. The resulting mixture was washed with 2*15 mL of sodium bicarbonate aq. and 2*10 mL of brine. The mixture was dried over anhydrous sodium sulfate and concentrated under vacuum. The residue was applied onto a silica gel column and eluted with ethyl acetate/petroleum ether (1:5). This resulted in 1.16 g (46%) of tert-butyl 4-(2-chloroethyl)piperazine-1-carboxylate as a off-white solid.

The synthetic route of 77279-24-4 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Ardelyx, Inc.; Lewis, Jason G.; Jacobs, Jeffrey W.; Reich, Nicholas; Leadbetter, Michael R.; Bell, Noah; Chang, Han-Ting; Chen, Tao; Navre, Marc; Charmot, Dominique; Carreras, Christopher; Labonte, Eric; (323 pag.)US9301951; (2016); B2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

5294-61-1, N-(2,6-Dimethylphenyl)-2-(piperazin-1-yl)acetamide is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,5294-61-1

To a solution of benzyl OXIRAN-2-YMETHYLCARBAMATE (12mmoles, 2. 5G) in ethanol (LOOML) was added triethylamine (24mmoles, 3. 34ML), followed by the addition of N- (2, 6- DIMETHYLPHENYL)-2-PIPERAZINYLACETAMIDE (24mmoles, 5.94g), a compound of formula (4). The resulting mixture was refluxed for 18 hours, then solvent removed from the reaction mixture under reduced pressure. The residue was purified by column chromatography on silica gel, eluting with 5% MEOH/DICHLOROMETHANE to give N-(2, 6-DIMETHYLPHENYL)-2-(4- {2-HYDROXY-3- [(PHENYLMETHOXY) carbonylamino] propyl} piperazinyl) acetamide, a compound of formula (5), as an off-white solid. Yield: 2.25g.

As the paragraph descriping shows that 5294-61-1 is playing an increasingly important role.

Reference£º
Patent; CV THERAPEUTICS, INC.; WO2004/63180; (2004); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

170911-92-9, tert-Butyl 4-(4-aminophenyl)piperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a stirred solution of 242 3-(2-chloro-6-fluoro-phenyl)-7-methylsulfanyl-2H-pyrimido[5,4-e][1,3]oxazin-4-one (150 mg, 0.462 mmol, 1.0 eq) in 24 toluene (3 mL) was added 25 m-CPBA (199 mg, 1.16 mmol, 2.5 eq) and allowed to stir at rt for 30 min. 66 Tert-butyl 4-(4-aminophenyl) piperazine-1-carboxylate (128 mg, 0.462 mmol, 1.0 eq) and 27 DIPEA (238 mg, 1.85 mmol, and 4.0 eq) were added and allowed to stir at rt for 1 h. Progress of reaction was monitored by LCMS. After completion of reaction, precipitated compound was filtered off and washed with toluene (2 mL) and dried under vacuum to afford 188 tert-butyl 4-[4-[[3-(2-chloro-6-fluoro-phenyl)-4-oxo-2H-pyrimido[5,4-e][1,3]oxazin-7-yl]amino]phenyl]piperazine-1-carboxylate (90 mg, 35.1%). LCMS: 555 [M+1]+, 170911-92-9

As the paragraph descriping shows that 170911-92-9 is playing an increasingly important role.

Reference£º
Patent; giraFpharma LLC; Chakravarty, Sarvajit; PHAM, Son Minh; Kankanala, Jayakanth; AGARWAL, Anil Kumar; PUJALA, Brahmam; SONI, Sanjeev; ARYA, Satish K.; PALVE, Deepak; KUMAR, Varun; (360 pag.)US2019/106436; (2019); 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.5747-48-8,11-(Piperazin-1-yl)dibenzo[b,f][1,4]thiazepine,as a common compound, the synthetic route is as follows.

Example 12 2-(2-(4-dibenzo[b,f][1,4]thiazepine-11-yl-1-piperazinyl)ethoxy)ethanol OR 11-[4-[2-(2-hydroxyethoxy)ethyl]-1-piperazinyl]dibenzo[b,f][1,4]thiazepine A 1 liter round bottom flask equipped with stirring rod, thermo pocket, water condenser was charged with solution of 11-piperazinyldibenzo[b,f][1,4]thiazepine in toluene 350 cc [63.0 g (0.22 moles)] and the mixture was stirred for 15 min 25-30 C., and was added sodium carbonate [41.0 gm (0.39 moles)], tetra butyl ammonium bromide [16.0 gm (0.05 mole)] and 2-(2-chloroethoxy)ethanol [32.0 gm (0.257 moles)] at room temperature. The reaction mixture was heated to reflux at 110-112 C. The reaction mixture was maintained at reflux for 10-12 hrs. The reaction mixture was analyzed by HPLC (to check for absence of compound of Formula IV) and was cooled to 25 C. to 30 C. To which, was added 150 cc DM water, then the reaction mixture was stirred for 30 min at 25-30 C. The layers were separated and the aqueous layer extracted with 50 cc toluene. The extract and the organic layer were combined, to which was added 250 cc water and was acidified with acetic acid to obtain a pH of 2-3. The reaction mixture was stirred for 30 min at 25-30 C. The layers were separated and the aqueous layer washed with 100 cc toluene twice. To the aqueous layer was added 250 cc toluene, and the pH was adjusted to 8-10 using sodium carbonate, the reaction mixture was stirred for 30 min at 25-30 C. The layers were separated and the aqueous layer extracted with 125 cc toluene. The extract and the organic layer were combined, to which was washed with DM (dimineralized) water 300 cc twice. The organic layer was distilled off under vacuum below 70 C. to afford 2-(2-(4-dibenzo[b,f]-[1,4]thiazepine-11-yl-1-piperazinyl)ethoxy)ethanol. Purity of 2-(2-(4-dibenzo[b,f]-[1,4]thiazepine-11-yl-1-piperazinyl)ethoxy)ethanol was 99.0% (area % by HPLC).

5747-48-8, As the paragraph descriping shows that 5747-48-8 is playing an increasingly important role.

Reference£º
Patent; Kansal, Vinod Kumar; Ahmad, Suhail; Lal, Kanhaiya; Patil, Bhatu Tumba; US2008/241949; (2008); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics