Category: piperazines

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 5 A reaction was carried out as described for Example 1, except that the solvent was changed from 44.7 g of 1-butanol to a mixed solvent consisting of 5.3 g of water and 40 g of 1-butanol (water content 10.6 wt%). After stirring at 0 to 5C for 2 hours, the reaction solution was analyzed. As a result, the reaction yield of 1-benzyloxycarbonyl-3-methylpiperazine was 82.1% (based on the amount of 2-methylpiperazine). Comparative Example 1 A reaction was carried out as described for Example 1, except that the solvent was changed from 44 g of 1-butanol to a mixed solvent consisting of 9 g of water and 35 g of 1-butanol (water content 20.5 wt%). After stirring at 0 to 5C for 2 hours, the reaction solution was analyzed. As a result, the reaction yield of 1-benzyloxycarbonyl-3-methylpiperazine was 59.6% (based on the amount of 2-methylpiperazine). Comparative Example 2 A reaction was carried out as described for Example 4, except that the solvent was changed from 44 g of 1-butanol to a mixed solvent consisting of 18 g of water and 27 g of 1-butanol (water content 40.0 wt%). After stirring at 0C for 2 hours, the reaction solution was analyzed. As a result, the reaction yield of 1-benzyloxycarbonyl-3-methylpiperazine was 51.6% (based on the amount of 2-methylpiperazine). Comparative Example 3 A reaction was carried out as described for Example 1, except that the solvent was changed from 44 g of 1-butanol to a mixed solvent consisting of 22 g of water and 22 g of 1-butanol (water content 50 wt%). After stirring at 0C for 2 hours, the reaction solution was analyzed. As a result, the reaction yield of 1-benzyloxycarbonyl-3-methylpiperazine was 33.6% (based on the amount of 2-methylpiperazine)., 109-07-9

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

Reference£º
Patent; Toray Fine Chemicals Co., Ltd.; EP1548010; (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.108-49-6,2,6-Dimethylpiperazine,as a common compound, the synthetic route is as follows.

1) Synthesis of cis-1-tert-butoxycarbonyl-3,5-dimethyl piperazine To an ethanol (42 ml) solution of 5.0 g (21.07 mmol.) of cis-3,5-dimethyl piperazine was added, at room temperature, 2.5 ml (32.3 mmol.) of di-tert-butyl dicarbonate. The mixture was stirred for one hour. The solvent was distilled off under reduced pressure. To the residue was added water, which was subjected to extraction with chloroform. The organic layer was washed with a saturated aqueous saline solution, which was dried over magnesium sulfate. The solvent was distilled off under reduced pressure to give the object compound as a pale yellow solid product. The yield was 5.77 g (72percent). 1H-NMR (CDCl3, 200 MHz) delta: 1.06 (6H, d, J=6.4 Hz), 1.46 (9H, s), 2.21-2.40 (2H, m), 2.68-2.86 (2H, m), 3.79-4.09 (2H, m). IR (KBr): 3319, 2972, 1680, 1425, 1367, 1315, 1267, 1173, 1144, 1072, 895, 866, 797 cm-1.

108-49-6, 108-49-6 2,6-Dimethylpiperazine 66056, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; Takeda Chemical Industries, Ltd.; US6235731; (2001); 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.55112-42-0,4-Methyl-1-piperazinecarbonyl Chloride Hydrochloride,as a common compound, the synthetic route is as follows.

55112-42-0, Example 7: Preparation of Zopiclone in acetonitrile[0070] To a slurry of 1 -chlorocarbonyl-4-methyl piperazine hydrochloride(CMP) (5.67g) in acetonitrile (ACN) (150 ml), mechanically stirred under nitrogen at O0C, were added Na2CO3 (4.98 g) and DMAP (0.46g) followed by addition of 7-OH- Py (5g). The reaction mixture was then stirred at 2C for 1.5h, under nitrogen followed by 18h stirring at room temperature and a few hours at reflux. After the reaction completion, the solvent was evaporated, to give a solid that was re-dissolved in Ethyl acetate and water. Phases were separated and the aqueous phase was extracted with Ethyl acetate. The solid formed in the aqueous layer was filtered to give zopiclone crude product (6.13g, yield 64.9%; purity 99.85% by HPLC).

55112-42-0 4-Methyl-1-piperazinecarbonyl Chloride Hydrochloride 3016934, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; TEVA PHARMACEUTICAL INDUSTRIES LTD.; TEVA PHARMACEUTICALS USA, INC.; WO2008/2629; (2008); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

5464-12-0, 1-(2-Hydroxyethyl)-4-methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

5464-12-0, A suspension of 60percent Sodium hydride in mineral oil (131.3 mg, 3.28 mmol) was washed with anhydrous hexane (5 mL) and suspended in anhydrous DMF (5 mL). l-(2- Hydroxyethyl)-4-methylpiperizine (473.6 mg, 3.28 mmol) was dissolved in DMF (5 mL) and added slowly to the above suspension at room temperature. The reaction mixture was stirred for 1 h at room temperature. Compound 99 (397 mg, 0.831 mmol) in DMF (5 mL) was slowly added to the reaction mixture. The reaction mixture was stirred for 3 h at room temperature. Ice water (25 mL) was added and the suspension was extracted with chloroform (2 x 100 mL). The solvent was removed under vacuum. After silica gel column chromatography (chloroform: methanol (9:1)), the resulting compound was dissolved in acetone (5 mL) and acidic solution (10 mL, acetone: 3N HCl (3:1)) was added. The reaction was stirred for 1 h at room temperature. The solvent was removed under vacuum and the pH was adjusted to 10 with concentrated ammonium hydroxide solution and extracted with chloroform (2 x 50 mL). The solvent was removed under vacuum. After silica gel column chromatography (methanol: cone, ammonium hydroxide (20:1)), the resulting compound was purified on alumina (dichloromethane: methanol (25:1)) to yield (CDD-0356) compound 113 (146 mg, 34.33percent) as a colorless oil. The free base CDD-0356 (113) was treated with fumaric acid in ethanol to yield the difumarate salt CDD-0356 (114) (130 mg) as white solid. CDD-0356F; 1H NMR (D2O): delta 1.49-1.67 (6H, m), 1.85-2.0 (4H, m), 2.26-2.32 (IH, m), 2.72 (3H, s), 2.76-3.6 (28H, m), 3.74-3.82 (IH, m), 4.26-4.34 (2H, m), 6.46 (4H, s).13C NMR (D2O/CD3OD): delta 19.05, 23.70, 24.22, 29.20, 29.61, 29.63, 29.7, 34.91, 34.93, 43.82(m), 47.3, 47.55, 50.1, 50.47 (m), 52.38 (m), 56.83, 56.85, 66.22 (m), 67.93, 67.97, 68.36, 68.37, 68.44, 68.48, 68.73, 68.74, 68.96, 135.73, 151.26, 163.31, 172.40. Anal: [C33H55N5Oi3S] C, H, N.

The synthetic route of 5464-12-0 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; UNIVERSITY OF TOLEDO; WO2009/152392; (2009); 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.103-76-4,N-(2-Hydroxyethyl)piperazine,as a common compound, the synthetic route is as follows.

103-76-4, [00212] Step 1 : To a solution of 4-fluoronitrobenzene (2.0g, 14.16 mmol) in AcN (15 mL), 2-(piperazin-l-yl)ethanol (1.85 g, 14.17mmol) and DIEA (2.97 mL, 17.01 mmol) were added. The mixture was refluxed for 15 h (in a sealed tube). After cooling, the resulting mixture was poured to water (300 ml). The mixture was stirred at room temperature for 30 min. The solids were collected by filtration and washed with water to afford the the desired product as off white solids (2.74g, 72% yield). ESI-MS calcd for (C12H17N303) 251, found 252 [M+H]+.

103-76-4 N-(2-Hydroxyethyl)piperazine 7677, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; NANTBIOSCIENCE, INC.; TAO, Chunlin; POLAT,, Tulay; WEINGARTEN, Paul; NALLAN, Laxman; ARP, Forrest; WANG, Qinwei; HO, David; (129 pag.)WO2016/138527; (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.2815-34-1,trans-2,5-Dimethylpiperazine,as a common compound, the synthetic route is as follows.

Diisopropylethylamine (0.38 ml) was added to a solution of tra?is-2,5-dimethyl- piperazine (1.50 g), phenyl acetic acid (0.59 g) and HATU (1.55 g) in DMF (10 ml). The reaction mixture was stirred overnight at ambient temperature. The solution was diluted with water, then extracted with ethyl acetate. The organic extracts were dried (MgSO4) then concentrated in vacuo to give the sub-title compound (1.8 g). EPO MS: APCI (+ve): 233 (M+l)

2815-34-1, 2815-34-1 trans-2,5-Dimethylpiperazine 220672, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2006/56752; (2006); 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

A mixture of compound 39a (250.0 mg, 0.591 mmol), N-isopropylpiperazine (113.8 mg, 0.887 mmol) and K2CO3 (251.1, 1.18 mmo) in DME (4.8 mL) is degassed with N2 for 15 min. After this time, bis(tri-t-butylphosphine)palladium(0) (30.2 mg, 0.059 mmol) is added and the reaction mixture is stirred at 100¡ã C. for 6 h. After this time, the reaction mixture is evaporated under reduced pressure, triturated with Et2O to give compound 39b (275 mg, 99percent).

4318-42-7, As the paragraph descriping shows that 4318-42-7 is playing an increasingly important role.

Reference£º
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; US2010/261714; (2010); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

934-98-5, 2-(4-Methylpiperazin-1-yl)ethanamine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A 250 mL round bottom flask equipped with a stir bar was charged with Example 1U (1.96 g) and anhydrous dichloromethane (160 mL) at room temperature under nitrogen. The mixture was cooled to 0¡ã C. in an ice bath, and 2-(4-methylpiperazin-1-yl)ethanamine (0.395 mL) was added via a syringe. The mixture was stirred for 25 minutes at 0¡ã C., and sodium triacetoxyborohydride (156 mg) was added as a solid. The reaction mixture was stirred for 15 minutes at 0¡ã C., and powdered activated 3 angstrom molecular sieves were added (1.96 g). The reaction mixture was stirred 2 hours at 0¡ã C., and was allowed to stir and warm slowly to room temperature overnight. LC/MS indicated one major peak with a mass that corresponded to desired product. The reaction mixture was quenched with dichloromethane and water. The layers were separated, and aqueous layer was extracted with dichloromethane and 10percent methanol/dichloromethane. The aqueous layer was neutralized with saturated aqueous NaHCO3 mixture, and was extracted one more time with 10percent methanol/dichloromethane. The combined extracts were washed with saturated aqueous NaHCO3 and brine, dried with Na2SO4, filtered, and concentrated. The residue was dissolved in dichloromethane and was purified on a Grace Reveleris X2 MPLC using a Teledyne Isco RediSep? Rf gold 750 g silica gel column eluting with a gradient of 0-20percent of methanol/dichloromethane over 40 minutes. The mixed fractions were purified on a Grace Reveleris X2 MPLC using a Teledyne Isco RediSep? Rf gold 330 g silica gel column eluting with a ramp of 0-15percent of methanol/dichloromethane over 40 minutes to collect additional title compound. The material from both columns was combined to provide the title compound. 1H NMR (501 MHz, dimethyl sulfoxide-d6) delta ppm 8.61 (m, 2H), 7.47 (m, 2H), 7.39 (d, 1H), 7.17 (m, 7H), 7.04 (td, 1H), 6.96 (dd, 1H), 6.67 (d, 1H), 6.51 (d, 1H), 5.84 (dd, 1H), 5.06 (m, 2H), 4.07 (ddq, 2H), 3.90 (d, 1H), 3.75 (s, 3H), 3.68 (dd, 2H), 3.50 (d, 1H), 3.17 (m, 1H), 3.08 (m, 1H), 2.90 (m, 2H), 2.65-2.20 (m, 10H), 2.14 (s, 3H), 1.67 (s, 3H), 1.09 (t, 3H). MS (ESI) m/z 928.4 (M+H)+., 934-98-5

The synthetic route of 934-98-5 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; AbbVie Inc.; AbbVie Deutschland GmbH & Co. KG; Brady, Patrick B.; Braje, Wilfried; Dai, Yujia; Doherty, George A.; Gong, Jane; Jantos, Katja; Ji, Cheng; Judd, Andrew S.; Kunzer, Aaron R.; Lai, Chunqiu; Mastracchio, Anthony; Risi, Roberto M.; Song, Xiaohong; Souers, Andrew J.; Sullivan, Gerard M.; Tao, Zhi-Fu; Teske, Jesse A.; Wang, Xilu; Wendt, Michael D.; Yu, Yiyun; Zhu, Guidong; Penning, Thomas D.; (218 pag.)US2019/55264; (2019); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

57260-71-6, tert-Butyl piperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

57260-71-6, The compound 1-tert-butoxycarbonyl piperazine (0.6g, 3.2mmol) and triethylamine (4.6mL, 32mmol) wasdissolved in dry tetrahydrofuran (10 mL), at room temperature, to this solution was added dropwisetrimethylsilyl isocyanate (4.2mL, 32mmol), stirred at rt for 1.5h, ice Water (10 mL), tetrahydrofuran spin, theaqueous phase with ethyl acetate (30mL ¡Á 3). The organic phase was dried over anhydrous Na 2 SO 4, removeThe solvent was concentrated and solid was washed with ethyl acetate (2mL) ultrasonic cleaning 1min, suctionfiltration, to give 0.3g white solid: 4-carbamoyl-piperazine 1-carboxylate, yield: 40%.

As the paragraph descriping shows that 57260-71-6 is playing an increasingly important role.

Reference£º
Patent; Guangdong East Sunshine Pharmaceutical Co., Ltd; Zhang, Ying jun; Liu, Bing; Yu, Tian Zhu; Zhang, Xiang Yu; (348 pag.)CN105399698; (2016); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

54699-92-2, 4-Methyl-1-piperazineacetic acid is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Example 13; General Method for the Preparation of Active Esters of N-Substituted Piperazine Acetic Acid from Trifluoroacetate Esters; A solution of the trifluoroacetate in THF (0.58 M, 1.2 equiv) was added to a solid sample of N-methyl piperazine acetic acid and mixed in a vortex or shaker until a homogeneous solution was obtained. The reaction of the carboxylic acid with the trifluoroacetate ester was generally complete within 30 min for all cases except N-hydroypyrrolidinone (NHP, 18 h). The progress of conversion to the active ester was monitored by ES-MS. The amount of product and any starting material (N-MPA) could be determined by direct infusion of a sample of the reaction (in ethanol) into the ES-MS. In some cases the active ester product was precipitated as dihydrochloride salt by the addition of a solution by addition of HCl solution in dioxane (4 M, 50% volume of the reaction) followed by washing with THF, ethyl acetate and hexanes. In other cases the product was isolated from the reaction as the mono TFA salt. Addition of TFA could be performed if the bis-TFA salt was desired. Dhbt ester, Calculated MH+ = 304.14 Found = 304.20 NHP ester, Calculated MH+ = 242.15 Found = 242.20 4-NP ester, Calculated MH+ = 280.13 Found = 280.20 1H NMR (400 MHz, CDCl3) d 8.20 (d, 2H, J=9.2 Hz, aromatic protons), 7.25 (d, 2H, J=9.2 Hz, aromatic protons), 3.69-3.40 (broad, 2H, ring protons), 3.57 (s, 2H, -CH2-CO-), 3.15-2.90 (broad, 6H, ring protons), 2.78 (s, 3H, -CH3). Pfp ester, Calculated MH+ = 325.10 Found = 325.10 Pcp ester, Calculated MH+ = 404.95 Found = 405.90 3-NP ester, Calculated MH+ = 280.13 Found = 280.20 NHS ester, Calculated MH+ = 256.13 Found = 256.10, 54699-92-2

As the paragraph descriping shows that 54699-92-2 is playing an increasingly important role.

Reference£º
Patent; Applera Corporation.; US2005/148771; (2005); A1;; ; Patent; Applera Corporation.; US2005/148774; (2005); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics