1-Methylpiperazine → N-(3,5-Dimethylphenyl)-2-[2-(4-methylpiperazin-1-yl)pyridin-4-ylmethylthio]pyridine-3-carboxamide

HRID 1984712

반응식

HRID 1984712 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.[CH3:8][C:9]1[CH:10]=[C:11]([NH:16][C:17]([C:19]2[C:20]([S:25][CH2:26][C:27]3[CH:32]=[CH:31][N:30]=[C:29](F)[CH:28]=3)=[N:21][CH:22]=[CH:23][CH:24]=2)=[O:18])[CH:12]=[C:13]([CH3:15])[CH:14]=1>C(OCC)(=O)C>[CH3:8][C:9]1[CH:10]=[C:11]([NH:16][C:17]([C:19]2[C:20]([S:25][CH2:26][C:27]3[CH:32]=[CH:31][N:30]=[C:29]([N:5]4[CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]4)[CH:28]=3)=[N:21][CH:22]=[CH:23][CH:24]=2)=[O:18])[CH:12]=[C:13]([CH3:15])[CH:14]=1

참가 물질

4

반응 조건

온도
150 °C

실험 절차

N-Methylpiperazine (2.0 mL) was added to N-(3,5-dimethylphenyl)-2-(2-fluoropyridin-4-ylmethylthio)pyridine-3-carboxamide (Reference compound No. 3-1, 100 mg, 0.27 mmol) at room temperature, then the vessel was sealed and the reaction mixture was stirred for 3 hours at 150° C. The mixture was cooled to room temperature, ethyl acetate (20 mL) was added to the reaction mixture, and then the whole was washed with brine (20 mL) and dried over anhydrous magnesium sulfate. The organic layer was evaporated under reduced pressure, and the resulting solid was filtered off with ethyl acetate to give 39 mg of the target compound as a colorless crystal. (Yield 32%)

후처리

  1. custom3-1, 100 mg, 0.27 mmol) at room temperature, then the vessel was sealed
  2. temperatureThe mixture was cooled to room temperature
  3. washthe whole was washed with brine (20 mL)
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe organic layer was evaporated under reduced pressure
  6. filtrationthe resulting solid was filtered off with ethyl acetate

출처 및 근거

ORD 기록
ord-4397937542924180b56feeef81aa8a17
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07544703B2

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