Tag: M.W:100-200

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

Example 24A 3-methyl-1-pyridin-2-ylpiperazine hydrobromide 2-Methylpiperazine (1.0 g, 0.01 mol, racemic mixture) and 2-bromopyridine (10 mL, 0.1 mol) were combined and heated at 120 C. for 16 hours. The reaction mixture was cooled to 23 C. and partitioned between ethyl acetate and water. The layers were separated, and the water layer was concentrated under reduced pressure. The residue was triturated with ethyl acetate, dichloromethane, and methanol to afford 460 mg (26% yield) of the title compound as an off-white solid. 1H NMR (300 MHz, DMSO-d6) delta 1.27 (d, J=6.6 Hz, 3H), 2.90 (dd, J=10.5, 14.1 Hz, 1H), 3.10 (m, 2H), 3.40 (m, 2H), 4.32 (m, 2H), 6.77 (dd, J=4.8, 6.9 Hz, 1H), 6.98 (d, J=8.1 Hz, 1H), 7.64 (m, 1H), 8.15 (m, 1H), 8.63 (bs, 1H), 8.92 (bs, 1H); MS (APCI) m/e 178 (M+H)+.

109-07-9, The synthetic route of 109-07-9 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Abbott Laboratories; US6960589; (2005); B2;,
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.75336-86-6,(R)-2-Methylpiperazine,as a common compound, the synthetic route is as follows.,75336-86-6

Example 1] Synthesis of compound (I-40) a) Synthesis compound 3 [Show Image] [Show Image] Under the nitrogen atmosphere, toluene (7.5 ml) was added to a commercially available compound 2 (1.50 g, 7.30 mmol), a commercially available compound 1 (1.50 g, 7-30 mmol), and sodium tert-butoxide (842 mg, 8.76 mmol) were added, and the system was degassed, and replaced with nitrogen. Xantphos (127 mg, 0.22 mmol) and Pd2(dba)3 (67 mg, 0.67 mmol) were added to react them at 100°C for 1 hour. Toluene (8 ml) was added to dilute the reaction, and this was filtered using Celite. The filtrate was concentrated under reduced pressure, and the resulting residue was purified by silica gel column chromatography (chloroform-methanol) to obtain a compound 3 (1.27 g, yield 77percent). 1H-NMR (CDCl3 / TMS) deltappm: 1.13 (d, J = 6.2Hz, 3H), 1.57 (s, 1H), 2.28-2.37 (m, 1H), 2.35 (s, 3H), 2.67 (dt, J = 3.5, 11.6Hz, 1H), 2.92-3.15 (m, 3H), 3.46 (d, J = 11.6Hz, 2H), 6.69 (dd, J = 8.9, 2.7Hz, 1H), 6.78 (d, J = 2.7Hz, 1H), 7.19 (d, J = 8.9Hz, 1H).

As the paragraph descriping shows that 75336-86-6 is playing an increasingly important role.

Reference：
Patent; Shionogi&Co., Ltd.; EP2184272; (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.59878-57-8,1-(Cyclopropylcarbonyl)piperazine,as a common compound, the synthetic route is as follows.

59878-57-8, In a 500 mL reaction flask, 2-fluoro-5-((4-oxo-3,4-dihydrophthalazin-1-yl)methyl)benzoic acid (Formula II, 15.0 g, 50.3 mmol) and DMF ( 100ml),After the addition, the system was stirred for 0.5 h to dissolve the system, and then 1-cyclopropyl-formylpiperazine (8.55 g, 55.4 mmol) and HBTU (21.0 g, 55.4 mmol) were added.DIPEA (8.5 g, 65.8 mmol) was then added dropwise to the system.The dropping process controls the reaction temperature not to be higher than 50 C, and the system is kept at 30 ± 5 C overnight after the addition.After the reaction was completed, the mixture was filtered, and the filter cake was washed with 1 L of purified water, and then the filter cake was transferred to a 1 L reaction flask.Purified water (500 mL) was added, kept at 30 ± 5 C, and stirred for 1 h.After suction filtration, the filter cake was washed with purified water (100 mL) and blast dried for about 24 h.The crude product (19.7 g) was obtained, and the crude material was recrystallized from DMF (75 ml)17.9g, 81.9%).

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

Reference：
Patent; Jiangsu Jun Ruo Pharmaceutical Co., Ltd.; Haimen Baikang Bio-pharmaceutical Co., Ltd.; Nanjing Jun Ruo Bio-pharmaceutical Institute Co., Ltd.; Wei Wanguo; Xu Zichen; Fang Xianjie; Zhu Xinlei; Liu Rufeng; Yi Mingyue; Zhou Chenglong; Liu Jie; Song Yaojie; (7 pag.)CN110078671; (2019); A;,
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.54699-92-2,4-Methyl-1-piperazineacetic acid,as a common compound, the synthetic route is as follows.,54699-92-2

Example 11; Synthesis of Active Esters Of N-Methyl Piperazine Acetic Acid Via Oxalyl Chloride (Scheme B, FIG. 4B); To a suspension of N-methyl piperazine acetic acid (N-MPAA) (79 mg, 0.5 mmol) in DCM (25 mL) was added a solution of oxalyl chloride (4 mL, 0.8 mmol, 2.0 M solution in DCM) over 10 minute at room temperature. After another 30 minutes of reaction, solvent and excess reagent were removed under reduced pressure to give a white solid (23). A solution of NHS (57 mg, 0.5 mmol) in DCM (25 mL) was added to the solid followed by ss-TBD (390 mg, 1 mmol, 2.6 mmol/g). The resulting solution was sonicated for 5 minute when all solid dissolved. The ss-TBD resin was removed by filtration and solvent was evaporated to yield a white foam (97% yield). Product was characterized by ES-MS as before.

The synthetic route of 54699-92-2 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Applera Corporation.; US2005/148773; (2005); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

17766-28-8, 1-Cyclohexylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

About 17.3kg of 4-((3-bromo-6-oxo-6H-anthra[l,9-cd]isoxazol-5- yl)amino)benzoic acid was mixed with about 238L of DMSO. About 11L of TEA and 12kg of 1-cyclohexyl piperazine were added to the reaction. Temperature was then raised to about 60- 65C. After 2-3 hours, slowly added about 116L of MTBE and MeOH (10: 1) solution and adjusted the temperature to 40-50C. The solid was centrifuged and washed by 22.5L of MTBE and MeOH (10: 1) solution and followed by about 22L of MeOH. Solid was dried under reduced pressure at about 25-30C for 12-24 hours. About 1.8kg phosphoric acid was dissolved in 90L of N-methyl pyrrolidone (NMP). Previously obtained crude product was dissolved in about 163L of NMP. Under about 40C, two solutions were mixed together for 1-2 hours. Then about 5.5kg of ECOSORB C-941 in about 20L of NMP was added to the previously mixed solution. The mixture was stirred for another 2- 3 hours under nitrogen protection before filtration. About 600L of purified water was slowly added to the solution under about 40C. Solid was centrifuged and washed with about 21L of water and followed by about 56L of MTBE. Solid was dried under reduced pressure at about 25- 30C for 8-12 hours to obtain the 4-((3 -(4-cyclohexylpiperazin- l-yl)-6-oxo-6H-anthra[ 1,9- cd]isoxazol-5-yl)amino)benzoic acid at about 98% purity and about 91% yield.

17766-28-8, As the paragraph descriping shows that 17766-28-8 is playing an increasingly important role.

Reference：
Patent; PURDUE PHARMA L.P.; WU, Jay Jie-Qiang; WANG, Ling; (31 pag.)WO2017/27465; (2017); 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.59702-07-7,1-Methylpiperazin-2-one,as a common compound, the synthetic route is as follows.

59702-07-7, [0808] To a solution of (8-((5-cyano-4-((2-methoxyethyl)amino )pyridin-2-yl)carbamoyl)-2-( dimethoxymethyl)-5,6, 7,8-tetrahydro-1 ,8-naphthyridin-3-yl)methyl methanesulfonate(intermediate 170, 368 mg, 0.657 mmol) in DCM(2.7 ml) at room temperature was added NEt3 (0.319 ml,2.301 mmol) followed by 1-methylpiperazin-2-one (120 mg,1.052 mmol). The reaction mixture was stirred at room temperaturefor 2 hand partitioned between DCM and water. Thewater layer was extracted multiple times with DCM, thecombined organic layers were dried using Na2S04 , filteredand evaporated. The crude product was purified by silica gelcolunm chromatography using a gradient ofMeOH (0-3percent) inDCM to yield the title compound as a white solid. (UPLC-MS3) tR 0.87 min; ESI-MS 553.3 [M+Ht. 1H NMR (600 MHz,CDCI3 ) ll13.75 (s, lH), 8.20 (s, lH), 7.64 (br s, lH), 7.58 (s,lH), 5.56 (s, lH), 5.23 (d, lH), 4.06-4.01 (m, 2H), 3.70 (br s,2H), 3.63 (t, 2H), 3.50-3.42 (m, 8H), 3.40 (s, 3H), 3.31 (br s,2H), 3.14 (br s, 2H), 2.96 (br s, 3H), 2.87-2.80 (m, 2H), 2.71(br s, 2H), 2.03-1.96 (m, 2H).

The synthetic route of 59702-07-7 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Novartis AG; Buschmann, Nicole; Fairhurst, Robin Alec; Furet, Pascal; Knoepfel, Thomas; Leblanc, Catherine; Liao, Lv; Mah, Robert; Nimsgern, Pierre; Ripoche, Sebastien; Xiong, Jing; Han, Bo; Wang, Can; Zhao, Xianglin; US2015/119385; (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.20327-23-5,1-Cyclopropylpiperazine,as a common compound, the synthetic route is as follows.

4-Cyclopropylmethyl-piperazine-1-carboxylic Acid 4-(5-trifluoromethyl-pyridin-2-yloxy)-phenyl Ester The hydrochloride of the title compound was prepared from 4-(5-trifluoromethyl-pyridin-2-yloxy)-phenyl chloroformate and 1-cyclopropylpiperazine, yield 62%. Recrystallisation from 0.2 M HCl gave white crystals, m.p. 238-239 C.; 1H NMR (DMSO-d6): delta 11.51 (br s, 1H), 8.61-8.55 (m, 1H), 8.30-8.20 (m, dd, 1H), 7.32-7.19 (m, d+s, 5H), 4.44-4.00 (br, 2H), 3.80-3.40 (br m, 4H), 3.29-2.93 (br m, 4H), 1.28-1.05 (br m, 1H), 0.75-0.58 (m, 2H), 0.50-0.35 (m, 2H).IR (KBr): nu 1730, 1713 (C=O) cm-1.

20327-23-5, The synthetic route of 20327-23-5 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Ebdrup, Soren; de Jong, Johannes Cornelis; Jacobsen, Poul; Hansen, Holger Claus; Vedso, Per; US2003/166644; (2003); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

75336-86-6, (R)-2-Methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

75336-86-6, To a solution of (R)-methylpiperazine (400 mg) in dichloromethane (20 mL) at 0 0C was added di-tert-butyl dicarbonate (871 mg). The reaction was stirred at room temperature for 4 h and then quenched with water (20 mL) and extracted into dichloromethane (2 x 40 mL). The combined organics were washed with saturated aqueous brine solution (40 mL), dried (MgSO4) and concentrated to give (R)-3-methyl-piperazine-l- carboxylic acid tert-butyl ester as a white solid (669 mg, 84%).

As the paragraph descriping shows that 75336-86-6 is playing an increasingly important role.

Reference：
Patent; PIRAMED LIMITED; GENENTECH, INC.; BAYLISS, Tracy; CHUCKOWREE, Irina; FOLKES, Adrian; OXENFORD, Sally; WAN, Nan, Chi; CASTANEDO, Georgette; GOLDSMITH, Richard; GUNZNER, Janet; HEFFRON, Tim; MATHIEU, Simon; OLIVERO, Alan; STABEN, Steven; SUTHERLIN, Daniel, P.; ZHU, Bing-Yan; WO2008/70740; (2008); 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.

EXAMPLE 41 4-(3-Methyl-1-piperazinyl)-1-(2-methylbenzenesulfonyl)-1H-indole (Scheme 1) The compound was prepared from 4-bromo-1-(2-methyl-benzenesulfonyl)-1H-indole and 3-methylpiperazine according to Method 1 to give 110 mg (38%) of a white solid: 1H-NMR (CD3OD) delta 7.92-6.82 (m, 9H), 3.64-3.39 (m, 5H), 3.12-3.03 (m, 1H), 2.92-2.83 (m, 1H), 2.47 (s, 3H), 1.40 (d, J=7 Hz, 3H); MS (ESI) 370.0 (M+H)+; Purity (HPLC) 94%.

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

Reference：
Patent; Caldirola, Patrizia; Nilsson, Bjorn M.; Johansson, Gary; US2002/165251; (2002); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

4318-42-7, 1-Isopropylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a solution of tert-butyl 4-hydroxypiperidine-1-carboxylate (4.4 g, 21.9 mmol) in 0CM (100 mL) was carefully added OMAP (5.3g, 43.Bmmol) and triphosgene (3.2g. 10.95 mmol) portionwise. After stirring at ft for 2h, 1-isopropylpiperazine (3.3g. 26 mmol) was added and the reaction mixture was stirred at ft for 5 h. The reaction was quenched with saturatedNH4CI (100 mL) solution and the mixture was extracted with 0CM (3×1 00 mL). The combined organic layers were washed with saturated NH4CI (2×100 mL) and brine (SOmL) sequentially, dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to afford thetitle compound as a white solid (7.7g. 99%). [LCMS: Rt1.67min, mz 356.3 (M + H)1., 4318-42-7

4318-42-7 1-Isopropylpiperazine 78013, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; NOVARTIS AG; AUBERSON, Yves; BOCK, Mark Gary; BRAGA, Dario; CURZI, Marco; DODD, Stephanie Kay; GIAFFREDA, Stefano Luca; JIANG, Haiyang; KARPINSKI, Piotr; TROXLER, Thomas J.; WANG, Tielin; WANG, Xiaoyang; ZHANG, Xuechun; WO2014/13469; (2014); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics