Month: April 2021

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.109-07-9,2-Methylpiperazine,as a common compound, the synthetic route is as follows.

To the 1200 L reactor was added [60C] racemic 2-methylpiperazine (100 kg) from a drum. H20 (240 L) was added, and the solution was cooled to [13C.] To the 1200 L receiver was added L-tartaric acid (150 kg). [H20] (140 L) was added, and the slurry was stirred for 1 h 35 min until dissolution of the solids was complete. The L-tartaric acid solution was transferred to the 1200 L reactor over 2 h while maintaining a temperature of [10-22C] in the 1200 L reactor followed by a [H20] rinse (20 L). Ethanol (163 kg) was added to the 1200 L reactor, and the solution was cooled to [2C.] The resulting slurry was stirred for 2 h at [2C,] and filtered through a 36″Nutsche filter sending the filtrate into the 1200 L receiver. The 1200 L reactor and 36″Nutsche filter were washed with H20 (200 L), and the solids were dried to yield 214 kg of 12% ee [(171%] based on the title compound). These solids were recharged to a clean 1200 L receiver and H20 (630 L) was added to the 1200 L receiver, which was heated to [85C] until all the solids had dissolved. The solution was filtered through an in-line filter (C) into the 1200 L reactor, cooled to [5C,] and stirred for 2 h. The resulting slurry was filtered through a clean 36″Nutsche filter sending the filtrate into the 1200 L receiver. The 1200 L reactor and 36″Nutsche filter were washed with [H20] (200 L), and the solids were dried to yield 104 kg of 93% ee (83% based on the title compound). These solids were recharged to a clean 1200 L receiver and [H20] (254 L) was added to the 1200 L receiver, which was heated to [85C] until all the solids had dissolved. The solution was filtered through an in-line filter (C) into the 1200 L reactor, cooled to [5C,] and stirred for 2 h. The resulting slurry was filtered through a clean 36″Nutsche filter sending the filtrate into the 1200 L receiver. The 1200 L reactor and 36″Nutsche filter were washed with H20 (200 L), and the solids were dried to yield 92 kg of 99% ee (74% based on the title compound). [D1] does not describe the preparation of the title compound but makes reference [TO J.] Med. Chem. 1990, 33, 1645-1656 (D2). The yield of the title compound according to D2, starting from racemic 2-methylpiperazine was 35%. M. Pt. 255.0-257. [0C.] ‘H NMR (400 MHz, [D20)] : [6] 4.79 [(D20,] reference), 4.36 (2H, s), 3.73-3. 64 (4H, [M),] 3.43 [(1H,] td J = 13.7, 3.0 Hz), 3.34 [(1H,] td, J = 12.7, 3.1 Hz), 3.17 [(1H,] dd, J = 14.2 12.8 Hz), 1.41 (3H, d, J = 6.1 Hz), 0.00 (TMS, reference). [13C] NMR (100 MHz, [D20)] : [6] 178.46 (s), 73.91 (d), 49.02 (d), 49.00 [(MEOH,] reference), 45.82 (t), 40.56 (t), 40.10 (t), 15.42 (q). IR (diffuse reflectance) 3426 (s), 3011 (s), 2999 (s), 2888 (s), 2785 (s, b), 2740 (s, b), 2703 (s, b), 2649 (s, b), 2483 (s, b), 2483 (s, b), 2361 (s), 2354,2340, 2248,1638 (s), cm HRMS (FAB) [CALCD FOR C5HL2N2 +HI 101.] 1079, found [101.] 1080. [[A]] [25D] = [24] (c 1.00, water). Anal. Calcd for [C4H606.] [C5HL2N2C,] 43.20 ; H, 7.25 ; N, 11.19. Found: C, 41.25 ; H, 7.45 ; N, 10.71.

109-07-9, As the paragraph descriping shows that 109-07-9 is playing an increasingly important role.

Reference£º
Patent; BIOVITRUM AB; WO2004/829; (2003); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

288251-85-4, tert-Butyl 4-(4-amino-2-cyanophenyl)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 21 3-(2,6-dichlorophenyl)-7-(methylthio)-2,3-dihydro-4H-pyrimido[5,4-e][1,3]oxazin-4-one (300 mg, 0.8767 mmol, 1.0 eq) in (10.0 mL) of 24 toluene was added 25 m-CPBA (376 mg, 2.1917 mmol, 2.5 eq) and allowed to stir at rt for 30 min followed by addition of 570 tert-butyl 4-(4-amino-2-cyanophenyl)piperazine-1-carboxylate (265 mg, 0.8767 mmol, 1 eq) and 27 DIPEA (452 mg, 3.506 mmol, 4.0 eq) and allowed to stir at rt for 12 h. The reaction mixture was diluted with water (50 mL) and extracted with EtOAc (2¡Á50 mL). The combined organic layers were washed with water (50 mL), brine (50 mL), dried over Na2SO4, concentrated and purified by flash chromatography (elution 0-35% 19 EtOAc in 20 Hexane) to afford the desired compound, 573 tert-butyl 4-(2-cyano-4-((3-(2,6-dichlorophenyl)-4-oxo-3,4-dihydro-2H-pyrimido[5,4-e][1,3]oxazin-7-yl)amino)phenyl)piperazine-1-carboxylate (150 mg, 28.68%) as an off white solid. (0600) LCMS: 596.2 [M+1]+, 288251-85-4

As the paragraph descriping shows that 288251-85-4 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.120737-59-9,tert-Butyl 3-methylpiperazine-1-carboxylate,as a common compound, the synthetic route is as follows.

Step 1: 1-BOC-3-Methylpiperazine (1.00 g) was combined with dichloromethane (10 mL), diisopropylethylamine (0.94 mL) and N-(benzyloxy-carbonyloxy)succinimide. The reaction was stirred at room temperature for 3 days and concentrated to dryness. The residue was diluted with ethyl acetate (20 mL) and washed with HCl (1 N in water, 3*5 mL), saturated aqueous sodium bicarbonate (3*5 mL) and brine (5 mL). The organic layer was dried over anhydrous magnesium sulfate, filtered and concentrated giving the desired benzyl carbamate. Yield=100percent, 120737-59-9

The synthetic route of 120737-59-9 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Millennium Pharmaceuticals, Inc.; US2003/153556; (2003); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

120737-59-9, tert-Butyl 3-methylpiperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

tert-butyl 3-methyl-4-(thiophen-2-ylsulfonvpipiperazine-1-carboxylate; Triethylamine (2.8 mL, 19.5 mmol) was added to a mixture of 2- chlorosulfonyl-thiophene (3.56 g, 19.5 mmol) and 3-methyl-piperazirie-1- carboxylic acid fert-butyl ester (3.90 g, 19.5 mmol) in DCM (50 mL). The reaction mixture was kept at room temperature for 1 hour under stirring (TLC monitoring, MeOH/CHCI3 5:95), washed with water, dried with sodium sulfate, and evaporated. The residue was purified by a silica gel column chromatography using EtOAc/n-hexane (2:1) as eluent to give tert-butyl 3- methyl-4-(thiophen-2-ylsulfonyl)piperazine-1-carboxylate (6.1 g, 90 percent). 1H NMR (DMSO-dbeta): 7.99 (dd, J = 5.1 Hz, J = 1.2 Hz, 1H); 7.67 (dd, J = 3.9 Hz1 J = 1.2 Hz, 1H); 7.22 (dd, J = 5.1 Hz, J = 3.9 Hz, 1H); 4.03 (mf 1H); 3.86 (br . signal, 1H); .3.67 (dm, J =13.0 Hz, 1H); 3.54 (dm, J = 13.0 Hz, 1H); 3.07 (m, 1H); 2.90 (br signal, 1H); 2.77 (br signal, 1H); 1.37 (s, 9H); 0.93 (d, J = 6.9 Hz, 3H)., 120737-59-9

Big data shows that 120737-59-9 is playing an increasingly important role.

Reference£º
Patent; TRIMERIS, INC.; WO2007/103456; (2007); A2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

3022-15-9, Piperazine-2-carboxylic acid dihydrochloride is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A solution of di-tert-butyldicarbonate (63 g, 290 mmol) in MeOH (100 mL) was added portionwise to a solution of piperazine-2-carboxyilic acid dihydrochloride (25.0 g, 123 mmol) and triethylamine (48 mL, 340 mmol) in MeOH (150 mL) over 30 minutes. Upon complete addition, the reaction mixture was heated to 50 0C for 2 h. Upon cooling to rt, the reaction mixture was concentrated under reduced pressure. The material was dissolved in water (300 mL) and the solution was brought to pH 2 with 1 M aqueous HCl. This was extracted with EtOAc (4 x 200 mL), and the combined extracts were dried over Na2SO4, filtered, and concentrated under reduced pressure until -100 mL EtOAc remained. The solution was diluted with hexanes (150 mL) and cooled to 0 0C. The resulting solid was collected by filtration, washed with hexanes (2 x) and air- dried. This gave 38.9 g (96%) of the title compound as a white solid. Analytical data: 1H NMR (400 MHz, DMSO-J6) delta 13.02-12.80 (br, IH), 4.50-4.24 (m, 2H)5 3.94-3.72 (br, IH), 3.66 (d, J= 12.8 Hz, IH), 3.22-2.92 (m, 2H), 2.90-2.68 (brs IH), 1.42-1.34, (m, 18H).

3022-15-9, The synthetic route of 3022-15-9 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; CRITICAL THERAPEUTICS, INC.; WO2007/146066; (2007); A2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

122833-04-9, 2-Methoxy-4-(4-methylpiperazin-1-yl)aniline is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a solution of 2,5-dichloro-N-(3-nitrophenyl)pyrimidin-4-amine (0.9 g, 3.16 mmol), 2-methoxy-4-(4-methylpiperazin-1-yl)benzenamine (0.7 g, 3.16 mmol), in 2-BuOH (20 mL) was added TFA (0.25 mL, 3.16 mmol) and the resultant slurry was refluxed for 8 hours. The reaction mixture was allowed to cool to room temperature, neutralized with a saturated aqueous sodium bicarbonate solution and then extracted with ethyl acetate (3*500 mL). The combined organic extracts were dried anhydrous Na2SO4, filtered and concentrated at reduced pressure to give an oil which was purified by column chromatography on silica gel (100-200 mesh) eluting with 1-2% (v/v) methanol in dichloromethane to furnish the title compound as a pale brown solid (1 g, yield 72%). 1H NMR 400 MHz (DMSO-d6) delta 9.16 (s, 1H), 8.48 (s, 1H), 8.21 (t, J=7.8 Hz, 1H), 8.11 (s, 1H), 8.02 (s, 1H), 7.88 (dd, J1=7.9 Hz, J2=2.4 Hz, 1H), 7.50-7.46 (m, 1H), 7.38 (d, J=8.8 Hz, 1H), 6.59 (d, J=2.4 Hz, 1H), 6.35 (dd, J1=8.8 Hz, J2=2.4 Hz, 1H), 3.74 (s, 3H), 3.12 (t, J=4.8 Hz, 4H), 2.49 (t, J=4.8 Hz, 4H), 2.24 (s, 3H); LCMS m/e: 470 [M+1]+.

122833-04-9, As the paragraph descriping shows that 122833-04-9 is playing an increasingly important role.

Reference£º
Patent; Sabila Biosciences LLC; MANSOUR, Tarek Suhayl; (66 pag.)US2018/208564; (2018); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

112257-12-2, tert-Butyl 4-(2-bromoacetyl)piperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A suspension of tert-butyl 4-(2-azidoacetyl)pipera-zine-1-carboxylate (2.92 g, 9.51 mmol) and sodium azide(1.54 g, 23.7 mmol) in CH3CN (47 mE) was refluxed for 1hour and cooled to room temperature. The reaction mixturewas diluted with EtOAc, washed with water and brine, driedover Na2504, filtered and concentrated in vacuo. The residuewas purified by recrystallization from EtOAc and hexanes toafford tert-butyl 4-(2-azidoacetyl)piperazine- 1 -carboxylate(2.28 g, 89%) as a white solid. ?H-NMR (CDC13, Varian, 400MHz): oe 1.47 (9H, s), 3.33-3.38 (2H, m), 3.42-3.50 (4H, m),3.58-3.66 (2H, m), 3.95 (2H, s)., 112257-12-2

As the paragraph descriping shows that 112257-12-2 is playing an increasingly important role.

Reference£º
Patent; HANDOK INC.; CMG Pharmaceutical Co., Ltd.; Kim, Moonsoo; Lee, Chaewoon; Lee, Gilnam; Yoon, Cheolhwan; Seo, Jeongbeob; Kim, Jay Hak; Lee, Minwoo; Jeong, Hankyul; Choi, Hyang; Jung, Myung Eun; Lee, Ki Nam; Kim, Hyun Jung; Kim, Hye Kyoung; Lee, Jae Il; Lee, MinWoo; Kim, Misoon; Choi, Soongyu; (124 pag.)US2016/168156; (2016); 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.

5747-48-8, ll-piperazinyldibenzo[b,f][l,4]thiazepine (100 g) was taken in n-butanol (600 ml). Sodium carbonate (53 g) and 2-chloroethoxyethanol (46 g) was added. The reaction mixture was heated to reflux at 110-120C for 10-12 hours. The reaction mixture was cooled and n-butanol was distilled off under vacuum. Ethyl acetate (600 ml) and water (500 ml) was added. The organic layer was separated off and the aqueous layer was first extracted with dilute hydrochloric acid and then basified with aqueous ammonia solution and extracted with ethyl acetate (800 ml). The organic layer was distilled off under vacuum to yield the title compound.

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

Reference£º
Patent; JUBILANT ORGANOSYS LIMITED; WO2006/27789; (2006); 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.109-07-9,2-Methylpiperazine,as a common compound, the synthetic route is as follows.

Reference Example 7 0.65 g of 2-methylpiperazine was added to a solution of 0.48 g of 1-cyclopropyl-6,7-difluoro-5-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylic acid in 5 ml of N-methyl-2-pyrrolidone, followed by heating at 90 C. for 20 minutes. After distilling off the solvent under reduced pressure, the residue was added with ethanol. The resulting crystals were filtered and recrystallized from ethyl acetate-ethanol to give 231 mg of 1-cyclopropyl-6-fluoro-7-(3-methyl-1-piperazinyl)-5-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylic acid. m.p.: 206 C.-208 C., white powder

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

Reference£º
Patent; Otsuka Pharmaceutical Co., Ltd.; US6333431; (2001); B1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

5625-67-2, Piperazin-2-one is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A 2-l Erlenmeyer flask was charged with 2-piperazinone (36.5 g, 364 mmol), sodium carbonate (116 g, 1.10 mol), 600 ml dioxane, and 150 ml water at room temperature. To this was slowly added benzyl chloroformate (62.1 g,364 mmol) over 20 min. After the addition was complete, the mixture was stirred for 2 h, diluted with water and extracted with 2 l of ethyl acetate. The combined organic extracts were dried (MgSO4), filtered and concentrated to give a white solid.To this solid was added 500 ml CH2Cl2, triethylamine (92.6 g, 128 ml, 911 mmol), 4-dimethylaminopyridine (4.45 g, 36.4 mmol), and di-tert-butyl dicarbonate (119 g,546 mmol). After 1 h at room temperature, the mixture was diluted with water and the organics were separated, dried (MgSO4), filtered and concentrated to give a brown oil. To this oil was added 100 ml CH2Cl2 followed by 1 l hexane. The resulting white solid was collected by filtration to give 4-benzyl 1-tert-butyl 2-oxo-1,4-piperazinedicarboxylate (101 g, 81%). 1H-NMR (400 MHz, CDCl3) delta 7.45-7.29 (m, 5 H), 5.15 (s, 2H), 4.24 (s, 2 H), 3.88-3.74 (m, 2 H), 3.74-3.59 (m, 2 H), 1.54 (s, 9H).

5625-67-2, The synthetic route of 5625-67-2 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Lloyd, David J.; St Jean, David J.; Kurzeja, Robert J. M.; Wahl, Robert C.; Michelsen, Klaus; Cupples, Rod; Chen, Michelle; Wu, John; Sivits, Glenn; Helmering, Joan; Komorowski, Renee; Ashton, Kate S.; Pennington, Lewis D.; Fotsch, Christopher; Vazir, Mukta; Chen, Kui; Chmait, Samer; Zhang, Jiandong; Liu, Longbin; Norman, Mark H.; Andrews, Kristin L.; Bartberger, Michael D.; Van, Gwyneth; Galbreath, Elizabeth J.; Vonderfecht, Steven L.; Wang, Minghan; Jordan, Steven R.; Veniant, Murielle M.; Hale, Clarence; Nature; vol. 504; 7480; (2013); p. 437 – 440;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics