Month: September 2020

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.31166-44-6,1-Cbz-Piperazine,as a common compound, the synthetic route is as follows.

31166-44-6, Dissolve compound 13 (500 g, 2.27 mol) in concentrated hydrochloric acid (1250 mL) And water (1250 mL),Then add sodium nitrite (469.89 g, 6.81 mol) dropwise at 25-30C within one hour.Dissolved in water (1000 mL) solution.The reaction was stirred at 25 C for 1 hour.TLC (petroleum ether: ethyl acetate = 1:1) showed complete reaction. The reaction was poured into ethyl acetate (2 L), the layers were separated and the aqueous layer was extracted with ethyl acetate (1 L x 2). The organic layers were combined, washed with 1 L of saturated brine, dried over anhydrous sodium sulfate, filtered, and concentrated to give the title compound 14 (yellow oil, 560 g, yield: 94.58%). It was used in the next step without purification.

31166-44-6 1-Cbz-Piperazine 643495, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; CHANGZHOU YINSHENG PHARMACEUTICAL CO., LTD.; FU, ZHIFEI; ZHANG, YANG; CHEN, SHUHUI; (29 pag.)TW2017/34011; (2017); A;,
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

A mixture of III-l-c (29 mg, 0.1 mmol), 2-methoxy-4-(4-methylpiperazin-l- yl)benzenamine (22 mg, 0.1 mmol), X-Phos (4.3 mg), Pd2(dba)3 (5.5 mg) and K2CO3 (41.5 mg, 0.3 mmol) in 1.2 mL of /-BuOH was heated at 100 C in a seal tube for 4 h. Then the reaction was filtered through celite and eluted with dichloromethane. Concentrated and the residue was purified by reverse-phase prep-HPLC using a water (0.05% TFA)/acetonitrile (0.05% TFA) gradient to afford the title compound HM as TFA salt (14 mg). 1H NMR (600 MHz, CD3OD) delta 8.03 (s, br, IH), 7.56-7.53 (m, 2H), 7.50-7.47 (m, IH), 7.36 (d, J = 7.2 Hz, 2H), 6.94 (d, J= 8.4 Hz, IH), 6.62 (s, IH), 6.08 (s, br, IH), 4.17 (t, J= 5.4 Hz, 2H), 3.84 (s, 3H), 3.78-3.72 (m, 2H), 3.63-3.58 (m, 2H), 3.35 (s, 3H), 3.28-3.22 (m, 2H), 3.06 (t, J= 4.8 Hz, 2H), 3.04-2.98 (m, 2H), 2.97 (s, 3H). MS (ESI) m/z 474 (M+H)+., 122833-04-9

The synthetic route of 122833-04-9 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; DANA FARBER CANCER INSTITUTE; GRAY, Nathanael, S.; DENG, Xianming; KWIATKOWSKI, Nicholas, Paul; WO2010/80712; (2010); A2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

259808-67-8, 1-Boc-3,3-Dimethylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

6-Chloro-8-isopropyl-imidazo [1 ,2-b]pyridazine-2-carboxylic acid (2.3 g, 9.5 mmol) was solubilized in N,N-dimethylformamide (37.8 mL) and DIPEA (3.06 g, 4.12 mL, 23.65 mmol). HATU (3.95 g, 10.4 mmol) was added followed by tert-butyl 3,3- dimethylpiperazine-1-carboxylate (2.23 g, 10.4 mmol). The solution was allowed to stir for 1 hour. Upon completion, a saturated aqueous solution of NH4C1 was added to the reaction mixture. The layers were partitioned and the aqueous layer was extracted 3 times with ethyl acetate. The combined organic layers were washed with brine, dried over anhydrous sodium sulfate, filtered and concentrated under vacuum. The crude product was purified by flash chromatography using 0-100% ethyl acetate: hexanes to afford the title compound (2.13 g, 51% yield). ?HNMR (400 MHz, Chloroform-d) oe 8.27 (s, 1H), 6.89 (s, 1H), 4.31 -4.17 (m, 2H), 3.67 – 3.45 (m, 5H), 1.63 – 1.58 (m, 6H), 1.51 – 1.46 (m, 9H), 1.44 – 1.37 (m, 6H). LCMS: mlz = 436.45 (M+Hj

259808-67-8, As the paragraph descriping shows that 259808-67-8 is playing an increasingly important role.

Reference£º
Patent; VERTEX PHARMACEUTICALS INCORPORATED; FARMER, Luc J.; FOURNIER, Pierre-Andre; LESSARD, Stephanie; LIU, Bingcan; ST-ONGE, Miguel; STURINO, Claudio; SZYCHOWSKI, Janek; YANNOPOULOS, Constantin; WO2015/48245; (2015); 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.148546-99-0,3-(4-Methylpiperazin-1-yl)aniline,as a common compound, the synthetic route is as follows.

Palladium acetate [Pd (OAc) 2] (10 mg, 0.022 mmol, 10%), (~)-BINAP (14 mg, 0.022 mmol, 10%) and dimethylformamide (4 mL) were charged in a round-bottom flask flushed with argon. The mixture was stirred under argon for 30 minutes. Then, 3- (4- METHYLPIPERAZIN-L-YL) phenylamine (84 mg, 0.44 mmol), 8-IODO-1-METHYL-N-[(LS)-2- morpholin-4-yl-1-phenylethyl]-4, 5-dihydro-1H-pyrazolo [4, 3-h]quinazoline-3- carboxamide (120 mg, 0.22 mmol), potassium carbonate (670 mg, 4.85 mmol) and dimethylformamide (1. 5 mL) were added. The resulting mixture was heated at 80C in an oil bath under argon with good stirring for 1.5 hours. After cooling to room temperature, the reaction mixture was poured into water and extracted with dichloromethane. The organic extracts were washed with brine and dried over NA2S04. The solvent was removed under vacuo, the crude was purified by flash chromatography on silica gel (eluant: dichloromethane/methanol 95: 5) to afford 40 mg (30% yield) of the title compound. IH NMR (400 MHz, DMSO-d6) 8 ppm 2.27 (s, 3 H) 2.52 (m, 8 H) 2.80 (t, 2 H) 2.94 (m, 4 H) 3. 13 (m, 4H) 3. 56 (m, 4H) 4. 39 (s, 3H) 5.16 (m, 1 H) 6. 59 (M, 1 H) 7. 14 (m, 1 H) 7.24 (m, 2 H) 7.33 (m, 2 H) 7.42 (m, 2 H) 8.39 (m, 2 H) 9.33 (s, 1 H)., 148546-99-0

As the paragraph descriping shows that 148546-99-0 is playing an increasingly important role.

Reference£º
Patent; PHARMACIA ITALIA S.P.A.; WO2004/104007; (2004); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

373608-48-1, tert-Butyl 4-(3-aminopropyl)piperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

JQ-acid (176.6 mg, 0.441 mmol, 1 eq) was dissolved in DMF (4.4 mL) at room temperature. HATU (176 mg, 0.463 mmol, 1.05 eq) was added, followed by DIPEA (0.23 mL), 1.32 mmol, 3 eq). After 10 minutes, tert-butyl 4-(3-aminopropyl)piperazine-1-carboxylate (118 mg, 0.485 mmol, 1.1 eq) was added as a solution in DMF (0.44 mL). After 24 hours, the mixture was diluted with half saturated sodium bicarbonate and extracted twice with DCM and once with EtOAc. The combined organic layer was dried over sodium sulfate, filtered and condensed. Purification by column chromatography (ISCO, 24 g silica column, 0-15% MeOH/DCM, 23 minute gradient) gave a yellow oil (325.5 mg, quant yield) (0663) 1H NMR (400 MHz, Chloroform-d) delta 7.67 (t, J=5.3 Hz, 1H), 7.41-7.28 (m, 4H), 4.58 (dd, J=7.5, 5.9 Hz, 1H), 3.52-3.23 (m, 8H), 2.63 (s, 9H), 2.37 (s, 3H), 1.80-1.69 (m, 2H), 1.64 (s, 3H), 1.42 (s, 9H). 13C NMR (100 MHz, cdcl3) delta 171.41, 164.35, 155.62, 154.45, 150.20, 136.92, 136.64, 132.19, 131.14, 130.98, 130.42, 129.98, 128.80, 80.24, 56.11, 54.32, 52.70, 38.96, 37.85, 28.42, 25.17, 14.43, 13.16, 11.82. LCMS 626.36 (M+H)., 373608-48-1

The synthetic route of 373608-48-1 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Dana-Farber Cancer Institute, Inc.; Bradner, James; Buckley, Dennis; Winter, Georg; (180 pag.)US2016/176916; (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, In 5 mL of acetonitrile was dissolved 500 mg (1.693 mmol) of 11-piperazin-l- yldibenzo[b,f][l,4]thiazepine. In 5 mL of acetonitrile at room temperature was dissolved H3PO4 (85% assay; 163 mg, 1.693 mmol). The solutions were combined resulting in immediate precipitation of a slightly gummy solid. The solid did not redissolve upon reheating, but did triturate into a free-flowing solid. There was no change upon standing overnight. The solids were collected, washed with acetonitrile (5 mL) and dried under vacuum at 40 0C resulting in 588 mg (88.7 %) of ciystalline solid, nip 227-233 0C (dec). 1H NMR (DMSO-d6) was consistent with the title salt.Polarized light microscopy revealed the material to be composed of rod-shaped crystalline particles. DSC revealed a series of endothermic events at higher temperatures likely corresponding to melting and degradation (see Figure 9). The TGA also indicated slight water loss of 0.5% at 105 0C (see Figure 9). DVS revealed that the material was slightly hygroscopic (see Figure 10). The moisture gain was reversible with some hysteresis on the first cycle (characteristic of a channel hydrate). The cycles overlapped well with no evidence of form change.

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

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

34334-28-6, 4-(4-Methylpiperazin-1-yl)benzonitrile is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

5-Nitro-furan-2-carboxylic acid 4-(4-methyl -piperazin-1-yl)-benzylamide (65). 5-Nitro-furan-2-carbonyl chloride (438 mg, 2.5 mmol) in CH2Cl2 (10 mL) was added to a mixture of crude amine 45b (410 mg, 2.0 mmol.) in Et3N (1.04 mL, 7.5 mmol) and the mixture was stirred for 12 hrs at room temperature. Reaction was carried out as explained above to afford 481 mg of amide 65 in 70% yields. 1H-NMR (500 MHz, CDCl3): delta 2.41 (3Hs, s), 2.63 (4Hs, t, J=4.88 Hz), 3.27 (4Hs, t, J=4.88 Hz), 4.6 (2Hs, d, J=5.61 Hz), 6.78-6.83 (1H, bs), 6.97 (2Hs, d, J=8.78 Hz), 7.31 (2Hs, d, J=8.78 Hz), 7.33 (1H, d, J=3.90 Hz), 7.41 (1H, d, J=3.90 Hz); 13C-NMR (300 MHz, CDCl3): ppm 41.71, 44.02, 48.06, 53.94, 111.31, 114.88, 115.52, 127.89, 128.91, 147.54, 149.95, 156.61; ESI-MASS: 345.3 (M+1); Anal. Calcd. for C17H2ON4O4: C, 59.29; H, 5.85; N, 16.27. Found: C, 59.16; H, 5.91; N, 16.19.

34334-28-6, As the paragraph descriping shows that 34334-28-6 is playing an increasingly important role.

Reference£º
Patent; University of Tennessee Research Foundation; US2005/222408; (2005); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

120737-78-2, tert-Butyl 2-methylpiperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A solution of 4,6-dimethyl-2-(o-tolyl)pyrimidine-5-carboxylic acid (26) (40 mg, 0.17 mmol), tert-butyl 2-methylpiperazine-1-carboxylate45 (50 mg, 0.25 mmol), HOBt(25 mg, 0.18 mmol), EDCI (28 mg, 0.18 mmol) and DIPEA (0.06 mL,0.33 mmol) in DCM (10 mL) was stirred at room temperature for18 h. The solution was then concentrated in vacuo before the residue was purified via silica gel chromatography (1:1 ethyl acetate/hexane) to afford compound 28, a clear oil (45 mg, 65%), as a mixture of conformers. Rf 0.44 (1:1 ethyl acetate/hexane). 1H NMR(CDCl3) d: 7.77e7.74 (m, 1H), 7.34e7.25 (m, 3H), 4.65 (m, 0.5H), 4.51 (m, 0.5H), 4.47 (m, 0.5H), 4.27 (m, 0.5H), 4.02 (m, 0.5H), 3.90 (m,0.5H), 3.40e3.32 (m, 1H), 3.21e2.95 (m, 3H), 2.59 (s, 1.5H), 2.57 (s,1.5H), 2.52 (s, 3H), 2.45 (s, 1.5H), 2.43 (s, 1.5H), 1.46 (s, 9H), 1.27 (d,J6.8 Hz, 1.5H), 1.12 (d, J6.8 Hz, 1.5H). 13C NMR (CDCl3) d: 168.1,167.8, 166.8, 166.8, 163.4, 162.8, 162.4, 154.41, 154.37, 137.9, 137.8,137.4, 137.3, 131.4, 131.43, 131.41, 130.38, 130.36, 129.64, 129.60,126.0, 125.8, 125.4, 80.6, 50.3, 46.9, 46.3, 46.2, 45.5, 41.5, 38.8, 38.0,28.5, 22.55, 22.50, 22.20, 22.15, 21.10, 21.08, 15.6, 15.5. To a solution of tert-butyl 4-(4,6-dimethyl-2-(o-tolyl)pyrimidine-5-carbonyl)-2-methylpiperazine-1-carboxylate (28) (45 mg,0.11 mmol) in DCM (3 mL) was added 10 drops of TFA and allowed to stir at room temperature for 18 h. The volatiles were evaporated to afford the product, a colourless oil (35 mg, quant.) as a mixture of conformers., 120737-78-2

120737-78-2 tert-Butyl 2-methylpiperazine-1-carboxylate 15087784, apiperazines compound, is more and more widely used in various fields.

Reference£º
Article; Lim, Zelong; Duggan, Peter J.; Wan, Soo San; Lessene, Guillaume; Meyer, Adam G.; Tuck, Kellie L.; Tetrahedron; vol. 72; 9; (2016); p. 1151 – 1160;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

259808-67-8, 1-Boc-3,3-Dimethylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

80.1: 4-(6-Methoxy-pyridine-2-carbonyl)-3,3-dimethyl-piperazine-1-carboxylic acid tert-butyl ester A mixture of 410 mg (2.28 mmol) 6-methoxy-2-pyridinecarboxylic acid and 400 muL (3.02 mmol) 1-chloro-N,N,2-trimethylpropenylamine in 10 mL THF was stirred at RT. After 1.5 h, 600 mg (2.66 mmol) 3,3-dimethyl-piperazine-1-carboxylic acid tert-butyl ester and 1.00 mL (5.81 mmol) DIPEA was added and the reaction mixture was stirred at RT for 30 min The reaction mixture was diluted with saturated NaHCO3 solution and extracted with EtOAc. The combined organic phases were dried over sodium sulfate, filtered and concentrated in vacuo. The crude material was purified by flash chromatography (PE/EtOAc=1/1).Yield: 780 mg (84%)ESI-MS: m/z=350 (M+H)+ Rt(HPLC): 1.23 min (method 3), 259808-67-8

259808-67-8 1-Boc-3,3-Dimethylpiperazine 22710387, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; HEIMANN, Annekatrin; DAHMANN, Georg; GRUNDL, Marc; MUELLER, Stephan Georg; WELLENZOHN, Bernd; US2013/158042; (2013); 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.5464-12-0,1-(2-Hydroxyethyl)-4-methylpiperazine,as a common compound, the synthetic route is as follows.

4-Nitropyrazole (2.81 g, 13.88 mmol) and 1-hydroxyethyl-4-methylpiperazine (1.0 g, 6.94 mmol) were dissolved in anhydrous tetrahydrofuran (50 mL), and a solution of triphenylphosphine (3.64 g, 13.88 mmol) and diisopropyl azodicarboxylate (2.81 g, 13.88 mmol) in anhydrous tetrahydrofuran (6 mL) was added dropwise under nitrogen gas atmosphere. The reaction solution was stirred at room temperature for 1 hour, and then 1N hydrochloric acid (30 mL) and water (50 mL) was added. The aqueous phase was extracted with ethyl acetate (50 mL*2). The combined organic phase was dried over anhydrous sodium sulfate, filtered and the filtrate was concentrated. The residue was purified by silica gel column chromatography (dichloromethane: methanol=10:1) to give compound 22-c (1.0 g, yield 60.2percent). LC-MS (ESI): m/z=240.2[M+H]+., 5464-12-0

As the paragraph descriping shows that 5464-12-0 is playing an increasingly important role.

Reference£º
Patent; GUANGZHOU MAXINOVEL PHARMACEUTICALS CO., LTD.; XU, Zusheng; ZHANG, Nong; WANG, Tinghan; SUN, Qingrui; WANG, Yuguang; (90 pag.)US2018/208604; (2018); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics