反応式
[NH2:1][CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:11]=[CH:10][N:9]=[CH:8][CH:7]=1.C(N(CC)CC)C.[C:19]1([C:24](Cl)=[O:25])[S:23][CH:22]=[CH:21][CH:20]=1>C(Cl)Cl>[C:19]1([C:24]([NH:1][CH2:2][CH2:3][CH2:4][O:5][C:6]2[CH:11]=[CH:10][N:9]=[CH:8][CH:7]=2)=[O:25])[S:23][CH:22]=[CH:21][CH:20]=1参加物
5
実験手順
To a solution of 700 mg (4.60 mmol) of 4-(3-aminopropyloxy)pyridine and 0.77 ml (5.52 mmol) of triethylamine in 30 ml of methylene chloride, 0.50 ml (4.68 mmol) of thenoyl chloride was added under ice-cooling with stirring. The mixture was stirred at room temperature for 1.5 hours. The reaction mixture was washed successively with a saturated aqueous solution of sodium bicarbonate and brine and dried over anhydrous magnesium sulfate, and the solvent was distilled off. The residue was purified by column chromatography (eluent: ethyl acetate) to obtain 850 mg of the desired compound (yield: 70.0%, colorless crystals).
後処理
- temperaturecooling
- stirringThe mixture was stirred at room temperature for 1.5 hours
- washThe reaction mixture was washed successively with a saturated aqueous solution of sodium bicarbonate and brine
- dry with materialdried over anhydrous magnesium sulfate
- distillationthe solvent was distilled off
- customThe residue was purified by column chromatography (eluent: ethyl acetate)
出典と根拠
- ORDレコード
- ord-6aaafa271c764cd7bffa5143f19ab4b3
- 出典データセット
- uspto-grants-1993_09
- 特許番号
- US05246948
関連ノート
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