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](Cl)(=[O:24])[C:20]([CH3:23])([CH3:22])[CH3:21]>C(Cl)Cl>[C:19]([NH:1][CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:11]=[CH:10][N:9]=[CH:8][CH:7]=1)(=[O:24])[C:20]([CH3:23])([CH3:22])[CH3:21]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, 0.57 ml (4.63 mmol) of pivaloyl 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 then the solvent was distilled off. The residue was purified by column chromatography (eluent: ethyl acetate) to obtain 840 mg of the desired compound (yield: 77.3%, 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-cc46162356544f669d9d762c2d76ff4b
- 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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