HRID358670

反应详情

EQUATION

反应方程式

HRID 358670 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-Hydroxy-1-methyl-4-quinolone (3 g) was suspended in dichloromethane (200 ml), triethylamine (5.6 ml) was added to the suspension and the mixture was stirred at ambient temperature for hour. 1 -Butanesulphonyl chloride (2.6 ml) was added to the suspension, the mixture stirred for 90 minutes and then left to stand overnight. The resultant mixture was washed with water (400 ml), aqueous sodium hydroxide (1M, 400 ml) and then further water (3×300 ml). The dichloromethane layer was dried over magnesium sulphate and evaporated to give a solid which was crystallised from methanol (100 ml) to give the novel compound 1-methyl-4-oxo-1,4-dihydroquinol-3-yl 1-butanesulphonate, m.p. 143°-144°.

WORKUP

后处理

  1. stirringthe mixture stirred for 90 minutes
  2. waitleft
  3. washThe resultant mixture was washed with water (400 ml), aqueous sodium hydroxide (1M, 400 ml)
  4. dry with materialThe dichloromethane layer was dried over magnesium sulphate
  5. customevaporated
  6. customto give a solid which
  7. customwas crystallised from methanol (100 ml)