Category: 109-01-3

109-01-3, 1-Methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

31.5 g of 4-chloro-1-nitrobenzene and 44.4 ml of 1-methyl-piperazine are combined and stirred for 18 hours at 90 C. Then the solution is poured onto ice water and the precipitate formed is suction filtered, washed with water and recrystallised from ethanol/water (1:1). The residue is dried in vacuo at 75 C. [00369] Yield: 44.0 g (99% of theory), [00370] Rf value: 0.5 (silica gel, methylene chloride/methanol=10:1) [00371] Melting point: 108-112 C., 109-01-3

The synthetic route of 109-01-3 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Boehringer Ingelheim Pharma GmbH & Co. KG; US6794395; (2004); B1;,
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.109-01-3,1-Methylpiperazine,as a common compound, the synthetic route is as follows.

To a 500 mL one-necked flask was added p-nitrobenzyl bromide (10 g, 46.3 mmol)And 100 mL of dichloromethane,4.7 g (47.0 mmol) of N-methylpiperazine was slowly added dropwise under ice-cooling (0-5 C)And triethylamine (7.1 g, 70.3 mmol)Of dichloromethane 20mL mixture, plus heat heating reflux 1h,TLC detected the disappearance of the starting material (ethyl acetate: petroleum ether = 1: 2).150 mL of chloroform and 100 mL of saturated sodium bicarbonate solution were added to the reaction solution,Stir for 30 min at room temperature. The reaction solution was extracted with chloroform (100 mL x 3)The organic layers were combined and washed once with water and saturated sodium chloride (100 mL x 1).Dried over anhydrous magnesium sulfate, filtered,The solvent was evaporated under reduced pressure to give 8.5 g of a pale yellow solid in a yield of 78.1%Products without further purification, directly into the next step.

109-01-3, The synthetic route of 109-01-3 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; China Pharmaceutical University; Lu Shuai; Wang Yue; Zhi Yanle; Yao Chao; Lu Tao; Li Baoquan; Chen Puzhou; Bao Jiyin; (27 pag.)CN107245073; (2017); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

109-01-3, 1-Methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A modified procedure of Mahesh et al, Pharmazie, 2005, 60, 6, 411-414, was used. After cooling a stirred solution of N-methylpiperazine (50 mmol, 5.55 ml) in 100 ml acetone to 0 C, 10 ml of an aqueous 25 % NaOH-solution and l-bromo-3-chloropropane (50 mmol, 7.87 g = 4.92 ml) were added cautiously. The reaction was stirred at RT for 24 hours. After concentrating the mixture under reduced pressure, the residue was diluted with water and extracted with dichloromethane. The collected organic phases were dried over Na2S04, filtered and concentrated. The residue was diluted with ethanol and after adding 2.3 M ethanolic HC1 l-(3-chloropropyl)-4-methylpiperazin-dihydrochloride crystallized as white crystals(12.5 mmol, 25 %). Mp = 257 C. ]H NMR (300 MHz, DMSO) 3.74 (t; 2H; 3J = 6.4 Hz; NCH7CH7CH7CI); 3.37 (m; 12H: NCH7CH7CH7Cl+4xpiperazin-CH7+2x H); 2.81 (s; 3H; CH3); 2.19 (d; 2H; J = 6.8 Hz; NCH2CH2CH2CI).

109-01-3, As the paragraph descriping shows that 109-01-3 is playing an increasingly important role.

Reference£º
Patent; JOHANNES GUTENBERG-UNIVERSITAeT MAINZ; DANNHARDT, Gerd; KRAMB, Jan-Peter; PLUTIZKI, Stanislav; WO2011/73092; (2011); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

109-01-3, 1-Methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Synthesis of 3-(4-methylpiperazin-1-yl)-propan-1-ol: 1-Methylpiperazine (6.99 mL, 63 mol) was dissolved in toluene (30 mL). 3-Bromopropanol (2.62 mL, 30 mmol) was added slowly and the mixture was stirred overnight at r.t. After heating to 80 C. for 2 h and cooling to r.t., the mixture was filtered and the filter cake was thoroughly washed with toluene. After removal of the solvent, the residue was subjected to Kugelrohr distillation (b.p., 180 C./2 mbar) to obtain a colourless oil (4.08 g, 25.8 mmol, 86%). LC/ESI-MS: m/z=159 [M+H]., 109-01-3

As the paragraph descriping shows that 109-01-3 is playing an increasingly important role.

Reference£º
Patent; 4SC AG; US2007/21446; (2007); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

109-01-3, 1-Methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

t-BOC-Protected methylpiperizine was heated in the presence of l-fluoro-4- nitrobenzene under pressure in benzene to give 4-t-BOC-protected 1-methyl-1- (4- nitrophenyl) piperazinium salt. The piperazinium salt was heated in the presence of potassium [F] fluoride and Krytofix at 200C for 10 minutes. The oil was treated with aq. 3 M HC1 for 20 minutes to give [F-18]-1-methyl-1-(4-fluorophenyl) piperazinium chloride, 109-01-3

As the paragraph descriping shows that 109-01-3 is playing an increasingly important role.

Reference£º
Patent; THE GENERAL HOSPITAL CORPORATION; WO2005/82425; (2005); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

109-01-3, 1-Methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Add 10 g (46.3 mmol) of p-nitrobenzyl bromide and 100 mL of dichloromethane to a 500 mL single-necked flask. A mixture of 4.7 g (47.0 mmol) of N-methylpiperazine and 7.1 g (70.3 mmol) of triethylamine in 20 mL of dichloromethane was slowly added dropwise under ice-water bath (0-5 C). After heating and refluxing for 1 hr, the material disappeared by TLC (ethyl acetate: petroleum ether = 1:2). 150 mL of chloroform and 100 mL of a saturated sodium hydrogencarbonate solution were added to the reaction mixture, and stirred vigorously at room temperature for 30 min. The reaction mixture was extracted with chloroform (100 mL¡Á3), and the organic layers were combined and washed with water and saturated sodium chloride (100 mL¡Á1). Dry over anhydrous magnesium sulfate, filter, The solvent was evaporated under reduced pressure to give 8.5 g of pale yellow solid. The yield was 78.1%, and the product was directly fed to the next reaction without further purification., 109-01-3

As the paragraph descriping shows that 109-01-3 is playing an increasingly important role.

Reference£º
Patent; Shanghai Fuxing Pharmaceutical Industrial Co., Ltd.; Lu Shuai; Jin Qiaomei; Wang Yue; Chen Yadong; Lu Tao; (54 pag.)CN104592251; (2019); B;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

109-01-3, 1-Methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: The mixture of 2a (1.9 g, 8.8 mM), morpholine (1.1 mL, 13.2 mM) and triethylamine (1.8 mL, 13.2 mM) were heated to reflux in THF for 2 h. The mixture was partitioned between ethyl acetate (60¡Á2 mL) and water (40¡Á2 mL), the organic layer was evaporated. The oily residue 3a utilized as materials without further purification., 109-01-3

As the paragraph descriping shows that 109-01-3 is playing an increasingly important role.

Reference£º
Article; Wang, Lu; Zhang, Qing; Zhu, Gaoyuan; Zhang, Zhimin; Zhi, Yanle; Zhang, Li; Mao, Tianxiao; Zhou, Xiang; Chen, Yadong; Lu, Tao; Tang, Weifang; European Journal of Medicinal Chemistry; vol. 130; (2017); p. 86 – 106;,
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.109-01-3,1-Methylpiperazine,as a common compound, the synthetic route is as follows.

A suspension of 2-chloro-/V-methyl-/V-(4-nitrophenyl)acetamide (1.0 g, 4.37 mmol) in ethyl acetate (10 mL) was heated to 40 C for 30 min and added l-methylpiperazine (1.2 mL, 10.9 mmol) at the same temperature. The mixture was stirred at 50 C for 2 h. The reaction mixture was cooled to RT and diluted with ethyl acetate. The solution was washed with water and dried over anhydrous sodium sulfate. The solution was filtered, concentrated and diluted with methanol. The solution was subjected to hydrogenation in the presence of palladium on carbon as catalyst under 25 bar of hydrogen pressure at 25 C for 2 h. The catalyst was removed by filtration and the solvent was evaporated at 60 C to yield 400 mg of the desired compound. 1 H NMR (400 MHz, DMSO-de) d 1.88 (s, 3H), 2.14-2.19 (m, 4H), 2.63-2.68 (m, 4H), 2.80 (s, 2H), 3.01 (s, 3H), 5.20 (br s, 2H), 6.53 (d, J= 8.1 Hz, 2H), 6.88 (d, J= 8.7 Hz, 2H)., 109-01-3

109-01-3 1-Methylpiperazine 53167, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; ICHNOS SCIENCES S.A.; CHAUDHARI, Sachin, Sundarlal; GHARAT, Laxmikant, Atmaram; IYER, Pravin; DHONE, Sachin, Vasantrao; ADIK, Bharat, Gangadhar; WADEKAR, Prashant, Dilip; GOWDA, Nagaraj; BAJPAI, Malini; (233 pag.)WO2020/70331; (2020); 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.109-01-3,1-Methylpiperazine,as a common compound, the synthetic route is as follows.

Intermediate 9: 3-(4-Methylpiperazin-1-yl)-propan-1-ol. 1-Methylpiperazine (6.99 mL, 63 mol) was dissolved in toluene (30 mL). 3-Bromopropanol (2.62 mL, 30 mmol) was added slowly and the mixture was stirred overnight at r.t.. After heating to 80C for 2 h and cooling to r.t., the mixture was filtered and the filter cake was thoroughly washed with toluene. After removal of the solvent, the residue was subjected to Kugelrohr distillation (b.p., 180C / 2 mbar) to obtain a colourless oil (4.08 g, 25.8 mmol, 86 %). 1H NMR (CDCl3): delta = 1.70 (Psi-quint, J ? 5.8 Hz, 2 H), 2.26 (s, 3 H), 2.35-2.6 (m, 8 H), 2.60 (Psi-t, J = 5.8 Hz, 2 H), 3.77 (Psi-t, J ? 5.3 Hz, 2 H), 4.09 (s, br., 1 H).

109-01-3, 109-01-3 1-Methylpiperazine 53167, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; 4SC AG; EP1674466; (2006); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

109-01-3, 1-Methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a solution of 4-fluorobenzonitrile (0.041 mol, 5 g) in DMF (10 ml) were added K2C03 (0.082 mol, 11.4 g) and 1 -methylpiperazine (0.062 mol, 6.15 g). The mixture was stirred over 1 8h at 100C. The mixture was partitioned between water and ethyl acetate. The organic phase was washed with water and brine. The resulting solution was dried oversodium sulfate and evaporated to dryness. The title compound was obtained as a white solid and used without further purification (7 g, 84%).(ESI+) MS: m/z 202.3 (MHj., 109-01-3

As the paragraph descriping shows that 109-01-3 is playing an increasingly important role.

Reference£º
Patent; EUDENDRON S.R.L.; UNIVERSITA’ DEGLI STUDI DI MILANO; ANGIOLINI, Mauro; ZUCCOTTO, Fabio; BERNARDI, Anna; AIRAGHI, Francesco; (144 pag.)WO2016/96709; (2016); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics