23 Sep 2021 News Downstream synthetic route of cis-2,6-Dimethylpiperazine

21655-48-1, The synthetic route of 21655-48-1 has been constantly updated, and we look forward to future research findings.

21655-48-1, cis-2,6-Dimethylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Add cis-2,6-dimethylpiperazine (1.0 g, 8.76 mmol) to a 100 mL single-mouth bottleAnd dichloromethane(20mL),Cool down to 0-5 C.Add triethylamine (2.22 g, 21.89 mmol),A solution of (Boc) 2O (1.92 g, 8.76 mmol) in dichloromethane (10 mL) was added dropwise.Warm to room temperature and stir overnight. The reaction was monitored by TLC. After the reaction was completed, the reaction mixture was concentrated under reduced pressure and purified by column chromatography.Eluent: DCM/MeOH = 30/1,The collected product was concentrated under reduced pressure to give 1.9 g.

21655-48-1, The synthetic route of 21655-48-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Beijing Purunao Bio-technology Co., Ltd.; Zhang Peilong; Shi Hepeng; Lan Wenli; Song Zhitao; (250 pag.)CN108707139; (2018); A;,
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Piperazines – an overview | ScienceDirect Topics

Sep 2021 News Downstream synthetic route of cis-2,6-Dimethylpiperazine

The synthetic route of 21655-48-1 has been constantly updated, and we look forward to future research findings.

21655-48-1, cis-2,6-Dimethylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

21655-48-1, (2S,6R)-2,6-dimethylpiperazine (6.85 g, 60.00 mmol) was added to ethyl 4-fluorobenzoate (2.201 mL, 15 mmol), in DMSO (40 mL) warmed to 120 C. under nitrogen. The resulting solution was stirred at 120 C. for 20 h. The reaction mixture was cooled and the solvent evaporated. The crude product was purified by silica column chromatography, eluting with a gradient of 0 to 10% methanol in dichloromethane containing 1% 880 ammonia. Pure fractions were evaporated to dryness to afford the desired compound (2.83 g, 71.9%) as a brown oil. 1H NMR (399.9 MHz, CDCl3) delta 1.15 (6H, d), 1.37 (3H, t), 2.38 (1H, d), 2.41 (1H, d), 2.96-3.04 (2H, m), 3.65-3.69 (2H, m), 4.33 (2H, q), 6.84-6.87 (2H, m), 7.89-7.93 (2H, m). MS: m/z 263 (MH+).

The synthetic route of 21655-48-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ASTRAZENECA AB; US2008/153812; (2008); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

23 Sep 2021 News New learning discoveries about 2-(4-Methylpiperazin-1-yl)ethanamine

934-98-5 2-(4-Methylpiperazin-1-yl)ethanamine 70284, apiperazines compound, is more and more widely used in various fields.

934-98-5,With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.934-98-5,2-(4-Methylpiperazin-1-yl)ethanamine,as a common compound, the synthetic route is as follows.

To a 10 ml RBF containing a magnetic stir bar was added 2-(4- Methylpiperazine-l-yl)ethanamine (143 mg, 1 mmol) in DCM (1 ml). Let stir under argon at room temperature. 1 , 1′-Carbonyldiimidazole (207 mg, 0.5 mmol) was added to the above solution using a spatula. Started forming a white precipitate. TLC on Sipsi2 in 100percent MeOH against the imidazolde indicated a very polar product.Let the solution stir overnight under argon. TLC indicated the completion of the reaction. Extracted the mixture into 25 ml EtOAc. Washed with 2×20 ml of distilled water and 20 ml brine. Combined the desired fractions and dried over anhydrous MgSOphi Filtered and concentrated in vacuo. Dissolved in the minimumamount of EtOAc and reprecipitated from hexanes. Filtered the product as a colorless solid and dried under vacuum to obtain a 69percent yield.eta and 13C NMR in CDCl3 with 2 drops of MeOD. Sample was designated NTF-2006-1-006A1FfNMR (300 MHz, CDCl3) 0.78 (t, J= 7.5 Hz, 3H), 1.08 (m, J= 7.5 Hz, 2H),1.38 (m, J= 7.5 Hz,4H), 1.47 (br s, 4H), 2.27 (s, 3H), 2.47 (br t,4H),2.54 (br t, 4H), 2.60 (t, J=6 Hz, 3H), 3.08 (m, J= 9.0 Hz, 2H), 3.52 (m, J= 5.7 Hz, 2H), 6.89 (d, J= 9.0 Hz, 2H), 7.07 (t, J= 6.9 Hz, IH), 7.28 (t, J= 8.4 Hz, 2H), 7.45 ( br d,J=1.8 Hz, IH), 7.55 (br d, IH) EPO 13C NMR (75 MHz, CDCl3) 14.00, 20,16, 31.32, 36.84, 43.26, 43.36, 46.23,53.07, 55.21, 56.99, 112.96, 115.64, 124.05, 130.44, 132.81, 136.18, 142.79, 142.84, 156.20FABMS 490 (M+H)+ ;HRMS calcd for 024H36N5O4S+ 489.2410 ; found 490.2510

934-98-5 2-(4-Methylpiperazin-1-yl)ethanamine 70284, apiperazines compound, is more and more widely used in various fields.

Reference:
Patent; FLYNN, Gary, A.; YOOL, Andrea, J.; MIGLIATI, Elton, Rodrigues; RITTER, Leslie, S.; WO2008/52190; (2008); A2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

23 Sep 2021 News Downstream synthetic route of 1-Isopropylpiperazine

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

4318-42-7,With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.4318-42-7,1-Isopropylpiperazine,as a common compound, the synthetic route is as follows.

General procedure: A mixture of the intermediates 3a-3e (5 mmol) and corresponding secondary amine 4a-4g (5.5 mmol) was added in CH3CN (20 ml) at the presence of anhydrous K2CO3 (6 mmol). The mixture was heated at 65 °C for 6-10 h. The solvent was evaporated in vacuo. The residue was dissolved in CH2Cl2 (25 mL), washed with water (20 mL × 3), and the combined organic phases were washed with saturated aqueous NaCl (30 mL), dried over sodium sulfate, and filtered. The solvent was evaporated under reduced pressure. The residue was purified on a silica gel chromatography using mixtures of petroleum/acetone as eluent to get the target products TM-1~TM-28.

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

Reference:
Article; Sang, Zhipei; Wang, Keren; Wang, Huifang; Yu, Lintao; Wang, Huijuan; Ma, Qianwen; Ye, Mengyao; Han, Xue; Liu, Wenmin; Bioorganic and Medicinal Chemistry Letters; vol. 27; 22; (2017); p. 5053 – 5059;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

23 Sep 2021 News Analyzing the synthesis route of 1-Cyclopropylpiperazine

20327-23-5 1-Cyclopropylpiperazine 4742004, apiperazines compound, is more and more widely used in various fields.

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.

Example B .22Preparation of compound (173) A mixture of compound (37), 1-cyclopropyl-piperazine (0.0027 mol), tris(dibenzylidene- acetone)dipalladium (0.054 mmol), l,r-[l,r-binaphthalene]-2,2′-diylbis[l,l-diphenyl- phosphine (0.081 mmol) and 2-methyl-propanol, sodium salt (1 :1) (0.00162 mol) in THF (5 ml) was stirred at 8O0C for 40 minutes under microwave. The mixture was filtered and concentrated to give the crude product. The crude product was purified by high-performance liquid chromatography (C 18, eluent: CH3CN / water from 8 / 92 to 38 / 62 with 0.1% CF3COOH ). The pure fractions were collected and the organic solvent was evaporated. The aqueous mixture was basified with solid NaHCOs to pH = 8. The aqueous mixture was extracted with DCM (40 ml) twice. The combined organic layers was washed with de-ion water (20 ml). The separated organic fraction was dried over sodium sulfate, filtered off the solid and the solvent was evaporated. The product was obtained by lyophilization, yielding 0.04 g of compound (173)., 20327-23-5

20327-23-5 1-Cyclopropylpiperazine 4742004, apiperazines compound, is more and more widely used in various fields.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; WO2009/132000; (2009); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Sep 2021 News Some tips on 1-Ethylpiperazine

5308-25-8 1-Ethylpiperazine 79196, apiperazines compound, is more and more widely used in various fields.

5308-25-8, 1-Ethylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

5308-25-8, A mixture of 4-amino-2-trifluoromethyl -benzoic acid (15 g, 73.1 mmol), HOBT (14.56 g, 95 mmol), EDC (16.82 g, 88 mmol), Et3N (20.38 mL, 146 mmol), 1-ethyl-piperazine (8.35 g, 73.1 mmol) in DCM (200 mL) was stirred at 25 C for 2 h. To the mixture was added DCM (200 mL) and then washed with H20, 2 M NaOH (2 x 150 mL) and brine. The organic layer was dried over NaaSOzi, filtered, and concentrated to give a off white solid of (4-amino-2-trifluoromethyl-phenyl)- (4-ethyl-piperazin-l-yl)-methanone (20 g, 65.2 mmol, 89.0% yield): NMR (400 MHz, CDC13) delta: 7.07 (d, J = 8.0 Hz, 1H), 6.92 (d, J = 2.4 Hz, 1H), 6.79 (dd, J = 2.0, 8.0 Hz, 1H), 3.99 (s, 2H), 3.84-3.76 (m, 2H), 3.25-3.23 (m, 2H), 2.50-2.39 (m, 4H), 2.33-2.31 (m, 2H), 1.08 (t, J = 7.2 Hz, 3H); ES-LCMS m/z 302 (M+H).

5308-25-8 1-Ethylpiperazine 79196, apiperazines compound, is more and more widely used in various fields.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; EIDAM, Hilary Schenck; DEMARTINO, Michael P.; GONG, Zhen; GUAN, Amy Huiping; RAHA, Kaushik; WU, Chengde; YANG, Haiying; YU, Haiyu; ZHANG, Zhiliu; CHEUNG, Mui; WO2014/141187; (2014); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Sep 2021 News Analyzing the synthesis route of 1-Cyclopentylpiperazine

21043-40-3 1-Cyclopentylpiperazine 806421, apiperazines compound, is more and more widely used in various fields.

21043-40-3, 1-Cyclopentylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Step A:6-Bromo-2-(4-cyclopentylpiperazin-1-yl)benzothiazole; To a solution of 6-bromo-2-chlorobenzothiazole (3 g, 12.1 mmol) in ethanol (50 mL) was added triethylamine (5.04 mL, 36.3 mmol) and 1-cyclopentylpiperazine (1.86 g, 12.1 mmol). The reaction mixture was heated at reflux for 16 h and then concentrated under reduced pressure. The residue was extracted with ethyl acetate and the combined organic extracts were washed with brine, dried (Na2SO4) and concentrated under reduced pressure to afford 4.3 g (99 %) of 6-bromo-2-(4-cyclopentylpiperazin-1-yl)benzothiazole., 21043-40-3

21043-40-3 1-Cyclopentylpiperazine 806421, apiperazines compound, is more and more widely used in various fields.

Reference:
Patent; NOVO NORDISK A/S; WO2007/110364; (2007); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Sep 2021 News Some tips on (R)-2-Methylpiperazine

75336-86-6, The synthetic route of 75336-86-6 has been constantly updated, and we look forward to future research findings.

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.

(R)-2-methylpiperazine (13.85 g, 138 mmol) and sodium bicarbonate (52.3 g, 622 mmol) were partially dissolved in a mixture of water (182 ml) and acetone (112 ml). A solution of benzoyl chloride (17.7 ml, 152 mmol) in acetone (56 ml) was added dropwise over 1 hour with vigorous stirring. After stirring for 16 hours at RT, the acetone was stripped on the rotovap, water (400 ml) was added, and the solution acidified (6M HCl) to a pH less than 2. The aqueous phase was washed three times with dichloromethane (200 ml) and then 5M sodium hydroxide was added to bring pH over 12. The resulting solution was extracted three times with dichloromethane (200 ml), dried (MgSO4) and evaporated to give (R)-(3- methylpiperazin-l-yl)(phenyl)methanone 62 as a yellow oil, 15.1 g (54percent of theoretical). LC/MS m/z = 205 (M+H+).

75336-86-6, The synthetic route of 75336-86-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; AMGEN INC.; WO2009/35568; (2009); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

Sep 2021 News Analyzing the synthesis route of 1-Methyl-3-phenylpiperazine

The synthetic route of 5271-27-2 has been constantly updated, and we look forward to future research findings.

5271-27-2, 1-Methyl-3-phenylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

5271-27-2, 1 -Methyl-3-phenylpiperazine (123.2 g; 0.70 mol) was dissolved in 500 dichloromethane. Triethylamine (30 ml; ca 0.2 mol) was added. A solution of ethyl chlorooxalate (107 g; 0.78 mol) in dichloromethane was slowly added under cooling. At 2/3 of the total addition a thick suspension was formed. Even after addition of more solvent, stirring remained difficult. The mixture was quenched with 10percent sodium carbonate. The organic layer is washed again with carbonate, dried and evaporated to an orange oil (191.2 g; 0.69 mol; 99 percent). Crystallisation with seeding proved difficult. Deep evaporation and storage as oil.TLC: very pure, a small amount of coloured polar material on baseline. No trace of the dioxamide (prepared from oxalylchloride and piperazine). GC: 18.0/18.2 min, 0.36 areapercent of 3.8 min impurity. A small sample (20 g) was stirred with water to induce crystallisation. mp ca 45 °C. The main bulk of the oil solidified after a few days of standing. Melting was needed before use.

The synthetic route of 5271-27-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; N.V. ORGANON; WO2007/144409; (2007); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

22 Sep 2021 News Simple exploration of tert-Butyl piperazine-1-carboxylate

The synthetic route of 57260-71-6 has been constantly updated, and we look forward to future research findings.

57260-71-6,With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.57260-71-6,tert-Butyl piperazine-1-carboxylate,as a common compound, the synthetic route is as follows.

A mixture of 4-iodoaniline (0.654 g, 3 mmol), piperazine-1-carboxylic acid tert-bvyl ester (0.67 g, 3.6 mmol), potassium phosphate (1.272 g, 6 mmol), ethylene glycol (0.33 ml) and copper iodide (0.03 g, 0.15 mmol) in 2-propanol (3 ml) was placed under argon in a sealed-tube and heated to 8O0C for 30 hours. After being cooled to room temperature, the medium was washed with water (50 ml) and extracted with ethyl acetate (100 ml). The organic layer was dried over MgSO4, concentrated and chromatographed (dichloromethane: acetone, 70:30) to yield 43a (0.36 g, 1.3 mmol, 43%) as a yellow powder.

The synthetic route of 57260-71-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; THE REGENTS OF THE UNIVERSITY OF CALIFORNIA; WO2006/124118; (2006); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics