Month: September 2021

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

Example 1 In a 100 ml four-neck flask, 5.00 g (= 0.0499 mole) of racemic 2-methylpiperazine was placed, and 44 g of 1-butanol (water content 0.05 wt%) was added for dissolution. The solution was cooled to 0C, and 8.47 g of benzyl chlorocarbonate (= 0.0489 mole, purity by HPLC determination analysis 98.5 wt%, 0.98 molar time) was added dropwise in a liquid temperature range from 0 to 8C. Then, stirring was carried out at 0 to 5C for 2 hours, and the reaction solution was partially sampled and determined by the internal standard method (internal standard: anisole). As a result, the reaction yield of 1-benzyloxycarbonyl-3-methylpiperazine was 83.9% (based on the amount of 2-methylpiperazine). The reaction solution was further stirred at room temperature for 12 hours and analyzed. As a result, the reaction yield was 85.1%. Example 3 A reaction was performed as described for Example 1, except that the amount of benzyl chlorocarbonate used was changed from 8.47 g to 10.1 g (= 0.0597 mole, 1.17 molar times). As a result, the reaction yield of 1-benzyloxycarbonyl-3-methylpiperazine was 93.8% (based on the amount of 2-methylpiperazine) after lapse of 2 hours at 0 to 5C. Stirring was carried out at room temperature for further 12 hours, being followed by analysis. As a result, the reaction yield was 95.1%., 109-07-9

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

Reference：
Patent; Toray Fine Chemicals Co., Ltd.; EP1548010; (2005); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

50606-32-1,50606-32-1, Butyl piperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

50.3. 4-[(R)-2-tert-Butoxycarbonylamino-3-(diethoxy-phosphoryl)-propionyl]-piperazine-l- carboxylic acid butyl ester: To a solution of intermediate 50.2 (7.37 g) in DCM (95 mL), THF (24 mL) and DIPEA (16.3 mL) were added HOBT (3.83 g) and EDC-HCl (4.78 g), and the reaction mixture was stirred at RT for 10 min. Subsequently, piperazine- 1 -carboxylic acid butyl ester (5.31 g) was added and the mixture stirred at RT for 2.5 h. The reaction mixture was diluted with DCM, the org. phase washed with sat. aq. NaHCO3 and the aq. phase re-extracted with DCM. The combined org. phases were washed with brine, dried over Na2SO^ and concentrated to dryness. Purification by CC (EtOAc/MeOH 1:0 to 9: 1) gave 7.66 g of the desired product. LC-MS: tR = 0.94 min; [M+H]+: 494.00

50606-32-1 Butyl piperazine-1-carboxylate 21963126, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; ACTELION PHARMACEUTICALS LTD; CAROFF, Eva; HILPERT, Kurt; HUBLER, Francis; MEYER, Emmanuel; RENNEBERG, Dorte; WO2010/116328; (2010); A2;,
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

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.112257-24-6,1-Boc-3-Carbamoylpiperazine,as a common compound, the synthetic route is as follows.,112257-24-6

A mixture of (S) -5- (1- ( (tert-butoxycarbonyl)amino) ethyl) -2- (3- (cyclopropylmethoxy) -4- (difluoromethoxy) phenyl)oxazole-4-carboxylic acid (300 mg, 0.64 mmol) , tert-butyl3-carbamoylpiperazine-1-carboxylate (153 mg, 0.64 mmol) , EDCI (250 mg, 1.3mmol) and HOAT (174 mg, 1.3 mmol) in DCM (25 mL) was stirred at 0 , and DIPEA(0.33 mL, 1.93 mmol) was added dropwise. After the addition, the mixture wasstirred at rt for 5 h and washed with water (10 mL × 3) . The organic layer wasdried over anhydrous Na2SO4 and concentrated. The residuewas purified by silica gel chromatography eluted with Petroleum ether/EtOAc(v/v) 2/3 to give the title compound as a white solid (220 mg, 50) . 1H NMR (400 MHz, CDCl3): delta ppm 7.52-7.61 (m, 2H) , 7.26 (d, J 8.3 Hz, 1H) , 6.72 (t, JF-H 75.0 Hz, 1H) , 5.42-5.49 (m, 1H) , 5.15-5.23 (m, 1H) , 4.01 (d, J 6.9 Hz,2H) , 3.71-3.79 (m, 1H) , 3.17-3.24 (m, 2H) , 1.59-1.64 (m, 3H) , 1.51 (s, 9H), 1.42 (m, 9H) , 1.30-1.35 (m, 1H) , 0.69-0.73 (m, 2H) , 0.42-0.45 (m, 2H) and MS-ESI: m/z 680.30 [M+H] +.

112257-24-6 1-Boc-3-Carbamoylpiperazine 11042527, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; SUNSHINE LAKE PHARMA CO., LTD.; ZHANG, Yingjun; LIU, Bing; YU, Tianzhu; ZHANG, Xiangyu; ZHANG, Shiguo; ZHANG, Jiancun; CHENG, Changchung; (426 pag.)WO2016/34134; (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.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

161357-89-7, 1-(Methylsulfonyl)piperazine hydrochloride is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

4-(5-Chloro-2-methyl-2,3-dihydro-furo[2,3-c]pyridin-2-yl)-piperidine-1-carboxylic acid tert-butyl ester (100 mg) is added to a mixture of 1-(methylsulfonyl)piperazine hydrochloride (70 mg), Pd2(dba)3 (65 mg), Xantphos (123 mg), and potassium tert-butylate (75 mg) in toluene (4 mL) under an argon atmosphere. The reaction mixture is stirred in an oil bath at 105 C. over night. After cooling to room temperature water is added and the mixture is extracted with ethyl acetate. The combined extracts are concentrated in vacuo and the residue is chromatographed on silica gel (cyclohexane/ethyl acetate 50:50?0:100) to give the title compound. LC (method 1): tR=1.03 min; Mass spectrum (ESI+): m/z=481 [M+H]+., 161357-89-7

The synthetic route of 161357-89-7 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; US2012/322784; (2012); 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.30459-17-7,1-(4-Trifluoromethylphenyl)piperazine,as a common compound, the synthetic route is as follows.

General procedure: Arylpiperazines (1.2 equiv) and potassium carbonate (4.0equiv) were added to a solution of 1 (1 equiv) in acetonitrile(CH3CN, 20 mL). The reaction mixture was heated to 85 Cand stirred for 12 h. Afterward the mixture was cooled toroom temperature. The reaction mixture was filtered, and thefiltrate was concentrated in vacuo. The residue was extractedwith ethyl acetate (60 mL) and water (20 mL). After dryingthe organic layer with anhydrous Na2SO4and evaporatingthe solvent under reduced pressure, a solid was appeared.The solid was recyrstallized from ethanol to obtain intermediates2.

30459-17-7, As the paragraph descriping shows that 30459-17-7 is playing an increasingly important role.

Reference：
Article; Chen, Hong; Jia, Huixia; Qian, Yuna; Shen, Jianliang; Yu, Yuzhong; Zhang, Haibo; Zhao, Shanchao; Pharmacological Reports; (2020);,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

548762-66-9, (2S,5R)-tert-Butyl 2,5-dimethylpiperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

(b) (2S,5R)-4-[5-(4-Bromo-3-trifluoromethoxy-phenylcarbamoyl)-pyridin-2-yl]-2,5-dimethyl-piperazine-1-carboxylic acid tert-butyl ester The product of the previous step (3.86 g, 10.2 mmol) (2S,5R)-2,5-dimethyl-piperazine-1-carboxylic acid tert-butyl ester (2.62 g, 12.2 mmol) and N,N-diisopropylethylamine (5.32 mL, 30.5) was dissolved in DMSO (12 mL). The reaction mixture heated at 120 C. for 3 h, diluted with EtOAc (100 mL), washed with water, and saturated NH4Cl, water, and brine. The reaction mixture was evaporated to about 40% volume and 3 M HCl in cyclopentyl methyl ether (4.24 mL, 12.7 mmol) was added slowly. Seeds from a previous run at smaller scale were added and the reaction mixture was stirred for 2 days and filtered to provide the HCl salt of the title intermediate (5.15 g, 83% yield). HPLC method C: Retention time=21.1 min

548762-66-9, As the paragraph descriping shows that 548762-66-9 is playing an increasingly important role.

Reference：
Patent; THERAVANCE, INC.; US2012/114600; (2012); 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.30459-17-7,1-(4-Trifluoromethylphenyl)piperazine,as a common compound, the synthetic route is as follows.

General procedure: To a stirred solution of 2-(3-bromopropyl) isoindoline-1,3-dione (1.0 g, 1 mmol) in N,N-dimethyl formamide DMF(5 mL), N-phenyl piperazine derivatives (1 mmol) andK2CO3 (1.1 g, 3 mmol) were added at room temperature.The reaction mixture was stirred at room temperature for 24h. The resulting solution was poured into ice cold water,which was then extracted with ethyl acetate. Ethyl acetatewas separated, dried over Na2SO4, and concentrated undervacuum to afford corresponding compounds 8a-g.

30459-17-7, 30459-17-7 1-(4-Trifluoromethylphenyl)piperazine 121718, apiperazines compound, is more and more widely used in various fields.

Reference：
Article; Venkatesh, Ramineni; Kasaboina, Suresh; Janardhan, Sridhara; Jain, Nishant; Bantu, Rajashaker; Nagarapu, Lingaiah; Medicinal Chemistry Research; vol. 25; 9; (2016); p. 2070 – 2081;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

262368-30-9, N-(4-Aminophenyl)-N-methyl-2-(4-methylpiperazin-1-yl)acetamide is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A solution of methyl (Z)-3-(chloro(4-(hydroxymethyl)phenyl)methylene)-2-oxoindoline- 5-carboxylate (17 mg, 0.05 mmol), N-(4-aminophenyl)-N-methyl-2-(4-methylpiperazin-1-yl)acetamide (15 mg, 0.06 mmol) and TEA (0.1 muL, 0.10 mmol) in EtOH (0.1 muL) was stirred under refluxed for overnight. The reaction solvent was evaporated under reduced pressure, and the residue was purified by column chromatography with dichloromethane/ethanol (50/1, v/v) to obtain the final compound 100 (15 mg, 52% yield): 1H NMR (500 MHz, DMSO-d6) _ 11.97 (s, 1H), 11.13 (s, 1H), 7.57 (d, J = 8.2 Hz, 1H), 7.51 (d, J = 7.8 Hz, 2H), 7.44 (d, J = 7.8 Hz, 2H), 7.13 (d, J = 8.2 Hz, 2H), 6.93 (d, J = 8.3 Hz, 1H), 6.90 (d, J = 8.2Hz, 2H), 6.51 (s, 1H), 5.49 (bs, 1H), 4.64 (s, 2H), 3.63 (s, 3H), 3.05 (bs, 2H), 2.69 (bs, 2H), 2.18 (bs, 6H), 2.10 (s, 3H); 13C NMR (125 MHz, DMSO-d6) _ 170.4, 168.6, 166.4, 157.2, 145.0, 140.4, 139.8, 130.3, 128.3, 127.8, 127.7, 127.0, 125.5, 124.0, 123.6, 121.3, 119.6, 108.8, 97.6, 62.4, 59.2, 54.6, 52.5, 52.4, 51.6, 51.5, 45.8, 36.7; HRMS (ESI-TOF) m/z calcd for C31H32N6O6 [M + H+] 569.2638 found 570.2713.

262368-30-9, The synthetic route of 262368-30-9 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; BOARD OF REGENTS, THE UNIVERSITY OF TEXAS SYSTEM; DALBY, Kevin N.; EDUPUGANTI, Ramakrishna; TALIAFERRO, Juliana; LEE, Juhyeon; (0 pag.)WO2018/160967; (2018); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics