Category: 13889-98-0

13889-98-0, 1-Acetylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A solution of 5.0 g (35.44 mmol) of 1-fluoro-4-nitrobenzene and 4.99 g (38.98 mmol) of N-acetylpiperazine in 50 mL of acetonitrile is heated at 60 C. for 15 hours. The resulting mixture is diluted with water and with ethyl acetate. After separation of the phases by settling and extraction of the aqueous phase with ethyl acetate, the organic phases are combined, dried over Na2SO4, filtered and concentrated under vacuum. 7.7 g of the expected product are obtained in the form of a yellow solid, which is used as obtained in the following step. Yield=88.8%., 13889-98-0

As the paragraph descriping shows that 13889-98-0 is playing an increasingly important role.

Reference：
Patent; SANOFI; US2012/277220; (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.13889-98-0,1-Acetylpiperazine,as a common compound, the synthetic route is as follows.

6-Bromopyridine-2-carboxaldehyde (2.0 g, 10.75 mmol) and 1-acetylpiperazine (6.9 g, 53.75 mmol) were dissolved in THF (120 ml). Upon cooling to O0C1 sodium triacetoxyborohydride (11.39 g, 53.74 mmol) was added to the reaction solution with a catalytic amount of HOAc. The mixture was slowly warmed to room temperature and was stirred at room temperature overnight. The suspension was filtered, and the filtrate was diluted with dichloromethane, washed with saturated aqueous sodium bicarbonate, dried over MgSO4 and concentrated to give a light color syrup. The syrup was purified by column chromatography, eluting with 10- 15% gradient of methanol in dichloromethane, to give 2.36 g (88%) of 1-acetyl-4-[(6- bromopyridin-2-yl)methyl]piperazine as a light color syrup. MS 298.1 (M+H); HPLC rt = 3.6 min [a].

13889-98-0, The synthetic route of 13889-98-0 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; WYETH; WO2009/76602; (2009); 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.13889-98-0,1-Acetylpiperazine,as a common compound, the synthetic route is as follows.

In a three neck flask, under inert atmosphere (N2), is added 7.19g (27.2mmol) ofD in 150ml of DCM. The mixture is cooled to 0C. Then 5.75g (30mmol) of EDCI, 4.05g (30mmol) of HOBt and 3.85g (30mmol) of acetylpiperazine are added in this order. The temperature of 0C is maintained for 1 hour and the mixture is allowed to warm to 20C over 18 hours. Then 50ml of water are added and a solution of HCl 1M is added to obtain an acidic aqueous phase. The solution is extracted with DCM. The crude product is purified by column chromatography (Eluant: 90/10 DCM/MeOH) to give 9.04g (yield=89%) of the title compound, Example 115, as a white solid. NMR 1H (DMSO d6) : delta 2.04 (s, 3H), 3.62-3.40 (m, 8H), 4.10-3.85 (m, 2H), 4.12 (d, 1H), 4.30 (d, 1H), 6.62 (t, 1HAr), 6.95 (d, 1HAr), 7.26 (d, 1HAr), 7.48 (t, 1HAr), 7.70 (m, 2HAr), 7.77 (s, 1HAr)., 13889-98-0

As the paragraph descriping shows that 13889-98-0 is playing an increasingly important role.

Reference：
Patent; CEPHALON, INC.; CEPHALON FRANCE; EP1586559; (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.13889-98-0,1-Acetylpiperazine,as a common compound, the synthetic route is as follows.

Example 12[4-(3,3-Bis-{4-[3-(4-acetyl-piperazin-1-yl)-prop-1-ynyl]-phenyl}allylsulfanyl)-2-methylphenoxy]acetic acidA mixture of 1-piperazin-1-yl-ethanone (15.2 g, 0.119 mol; prepared as described in U.S. Pat. No. 2,973,362), 3-bromopropyne (17 g, 0.143 mol) and potassium carbonate anhydrous (21.5 g, 0.156 mol) in 2-butanone (150 mL) was refluxed for 6 h. A separated solid was filtered off, washed with 2-butanone (80 mL) and 2-butanone was evaporated in vacuo. The residue was purified by vacuum distillation to yield 1-(4-prop-2-ynylpiperazin-1-yl)ethanone, b.p. 115 C./7 Torr).Yield: 12.2 g (62%).M.p. 63-65 C.

13889-98-0, 13889-98-0 1-Acetylpiperazine 83795, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; Novo Nordisk A/S; High Point Phamaceticals LLC; US2011/39841; (2011); 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.13889-98-0,1-Acetylpiperazine,as a common compound, the synthetic route is as follows.

General procedure: A reaction vessel was charged with acetic acid (2.016 mmol) and TBHP (70% inwater, 1.008 mmol) in acetonitrile (2 mL). After the addition of [Bpy]I (0.1008 mmol),benzoxazole (0.672 mmol) and secondary amines (1.344 mmol) were added. Then thereaction mixture was stirred at room temperature for 3.5 hours. After the reactionfinished, the mixture was extracted with dichloromethane (5 × 10 mL), and thecombined organic phases were dried over anhydrous Na2SO4. The solvent wasevaporated under vacuo, and the crude residue was purified by columnchromatography on silica gel. Aqueous phase was dried in a vacuum evaporator torecover the ionic liquid and directly reused in subsequent runs., 13889-98-0

As the paragraph descriping shows that 13889-98-0 is playing an increasingly important role.

Reference：
Article; Zhou, Ya; Liu, Zhiqing; Yuan, Tingting; Huang, Jianbin; Liu, Chenjiang; Molecules; vol. 22; 4; (2017);,
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.13889-98-0,1-Acetylpiperazine,as a common compound, the synthetic route is as follows.

A mixture of N-[4-(2-Bromo-ethoxy)-3-(2-methyl-2H-pyrazol-3-yl)-phenyl]-3-methoxy-benzamide (90 mg, 0.21 mmole), and 1-Piperazin-1-yl-ethanone (32 mg, 1.2 eq), and K2CO3 (116 mg, 4.0 eq) in 2 mL DMF was stirred at 120 C. for 20 minutes in microwave. The mixture was purified by HPLC to give title compound as a white solid as TFA salt (97 mg, 97%). 1H NMR (Acetone-d6, 400 MHz) delta 2.07 (s, 3H), 3.30 (sb, 4H), 3.71 (t, J=4.80 Hz, 2H), 3.75 (s, 3H), 3.79 (sb, 2H), 3.87 (s, 3H), 4.60 (t, J=4.80 Hz, 2H), 4.99 (sb, 2H), 6.32 (s, 1H), 7.13 (d, J=8.08 Hz, 1H), 7.23 (d, J=9.09 Hz, 1H), 7.42 (t, J=8.08 Hz, 1H), 7.53 (m, 2H), 7.56 (d, J=7.83 Hz, 1H), 7.82 (s, 1H), 7.94 (dd, J=8.84, 2.53 Hz, 1H), 9.56 (s, NH). Exact mass calculated for C26H31N5O4477.2, found 478.3 (MH+).

13889-98-0, 13889-98-0 1-Acetylpiperazine 83795, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; Teegarden, Bradley; Xiong, Yifeng; Strah-Pleynet, Sonja; Jayakumar, Honnappa; Dosa, Peter I.; Feichtinger, Konrad; Casper, Martin; Lehmann, Juerg; Jones, Robert M.; Unett, David J.; Karoline Choi, Jin Sun; US2007/207994; (2007); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

13889-98-0, 1-Acetylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,13889-98-0

(0452) 1-(Piperazin-1-yl)ethan-1-one (2.56 g, 20 mmol) and 4-fluoro-2-methoxy-1-nitrobenzene (3.42 g, 20 mmol) were dissolved in N,N-dimethylformamide (30 mL), and potassium carbonate (5.52 g, 40 mmol) was added. The reaction was carried out at 70 C. for 16 h. The reaction solution was cooled to room temperature, and poured into water (150 mL). The mixture was extracted with ethyl acetate (150 mL×4), and the water phase and the organic phase was separated. The organic phases were combined, washed with saturated saline solution, dried with anhydrous sodium sulfate, and concentrated. The crude product was purified by silica gel column chromatography (ethyl acetate: petroleum ether=1:10-2:1) to get the title compound as a light yellow solid (4.8 g, yield: 86.0%).

The synthetic route of 13889-98-0 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Xuanzhu Pharma Co., Ltd.; WU, Frank; (117 pag.)US2017/112833; (2017); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

13889-98-0, 1-Acetylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,13889-98-0

INTERMEDIATE 10( S)-ter t-Butyl 1 – |~2-(4-acetylpiperazin- 1 -yl)-7-fluoro-8-methylquinolin-3 – yl 1 ethylcarbamateIntermediate 9 (3.0 g, 0.89 mmol) in NMP (15 mL) was treated with 1 -acetyl – piperazine (2.8 g, 22 mmol) and DIPEA (5.7 g, 44 mmol) and heated in a sealed tube at 140C for 72 h. The reaction mixture was cooled to r.t. and diluted with ethyl acetate/ water. The organic phase was washed (water, brine), dried (phase separation cartridge) and evaporated in vacuo. The resulting residue was purified by silica flashchromatography, eluting with 50-60% EtOAc in isohexane, to give the title compound (3.4 g 89%) as a cream solid. deltaEta (CDC13) 7.95 (1H, s), 7.53 (1H, dd, J 8.9, 6.0 Hz), 7.16 (1H, t, J 8.9 Hz), 5.08-5.02 (1H, m), 3.95-3.90 (1H, m), 3.78-3.73 (2H, m), 3.64 (1H, m), 3.61-3.40 (2H, m), 3.19-3.15 (2H, m), 2.59 (3H, d, J2.4 Hz), 2.17 (3H, s), 1.58 (3H, d, J 6.5 Hz), 1.48-1.42 (9H, m).

As the paragraph descriping shows that 13889-98-0 is playing an increasingly important role.

Reference：
Patent; UCB PHARMA S.A.; BUeRLI, Roland; HAUGHAN, Alan, Findlay; MATTEUCCI, Mizio; OWENS, Andrew, Pate; RAPHY, Gilles; SHARPE, Andrew; WO2011/58110; (2011); 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.13889-98-0,1-Acetylpiperazine,as a common compound, the synthetic route is as follows.

4-Fluorobenzaldehyde15 (619 muL, 5.85 mmol), 1-acetylpiperazine (500 muL, 3.90 mmol) and Na2CO3 (620 mg, 5.85mmol) were dissolved in H2O (25 mL) and the stirred at 100C overnight. After extractionwith DCM, the combined organic layers were concentrated under reduced pressure and silicagel column chromatography (3% MeOH/DCM) yielded 17a (942 mg, 58%). 1H NMR (500MHz, DMSO-d6) delta 9.73 (s, 1H), 7.73 (d, J = 8.9 Hz, 2H), 7.04 (d, J = 8.9 Hz, 2H), 3.65-3.54 (m,4H), 3.50-3.44 (m, 2H), 3.42-3.36 (m, 2H), 2.04 (s, 3H); 13C NMR (126 MHz, DMSO-d6) delta190.2, 168.42, 154.3, 131.4, 126.4, 113.2, 46.3, 46.0, 44.9, 40.3, 21.1; HRMS (ESI-MS): Calculatedfor C13H17N2O2 [M+H]+: 233.12845; found: 233.12871.

13889-98-0, 13889-98-0 1-Acetylpiperazine 83795, apiperazines compound, is more and more widely used in various fields.

Reference：
Article; Buehrmann, Mike; Wiedemann, Bianca M.; Mueller, Matthias P.; Hardick, Julia; Ecke, Maria; Rauh, Daniel; PLoS ONE; vol. 12; 9; (2017);,
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.13889-98-0,1-Acetylpiperazine,as a common compound, the synthetic route is as follows.

13889-98-0, Example 83 1-acetyl-4-{[2-(5-{1-[4-(methylsulfonyl)phenyl]-2-(tetrahydro-2H-pyran-4-yl)ethyl}-1H-pyrrol-2-yl)pyridin-4-yl]methyl}piperazine To a solution of 2-(5-{1-[4-(methylsulfonyl)phenyl]-2-(tetrahydro-2H-pyran-4-yl)ethyl}-1H-pyrrol-2-yl)pyridine-4-carbaldehyde (170 mg) in 1,2-dichloroethane (5 mL) was added 1-acetylpiperazine (115 mg), and the mixture was stirred at room temperature for 30 min. To the reaction mixture was added sodium triacetoxyborohydride (250 mg), and the mixture was stirred overnight at room temperature. The reaction mixture was diluted with ethyl acetate, washed with saturated aqueous sodium hydrogen carbonate and saturated brine, dried (MgSO4) and concentrated. The residue was subjected to basic silica gel column chromatography, and the title compound (180 mg, yield 85%) was obtained as a pale-yellow amorphous solid from a fraction eluted with ethyl acetate-methanol (19:1, volume ratio). MS:551(MH+). 1H NMR (300 MHz, CDCl3) delta1.29 – 1.50 (3 H, m), 1.54 – 1.60 (1 H, m), 1.82 – 1.97 (1 H, m), 2.08 (3 H, s), 2.36 – 2.50 (4 H, m), 3.04 (3 H, s), 3.20 – 3.37 (2 H, m), 3.40 – 3.53 (4 H, m), 3.58 – 3.69 (2 H, m), 3.86 – 3.99 (2 H, m), 4.14 – 4.22 (1 H, m), 6.15 (1 H, t, J=3.0 Hz), 6.59 – 6.72 (1 H, m), 6.93 – 7.06 (1 H, m), 7.36 – 7.53 (3 H, m), 7.87 (2 H, d, J=8.3 Hz), 8.32 (1 H, d, J=4.5 Hz), 9.28 (1 H, brs).

The synthetic route of 13889-98-0 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Takeda Pharmaceutical Company Limited; EP2149550; (2010); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics