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

HRID 1984712

反応式

[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

参加物

反応条件

温度: 150 °C

実験手順

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%)

後処理

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

出典と根拠

ORDレコード: ord-4397937542924180b56feeef81aa8a17
出典データセット: uspto-grants-2009_06
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US07544703B2

反応式

参加物

反応物 2

生成物 1

試薬・触媒・溶媒 1

反応条件

実験手順

後処理

出典と根拠

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