HRID1109612

反应详情

EQUATION

反应方程式

HRID 1109612 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 0.5 g (0.0037 mole) of 5-chloro-3-hydroxyisothiazole and methyl vinyl ketone (1.0 g, 0.014 mole) in 15 ml of toluene was heated at 80° C. for 24 hours. After cooling and removal of toluene and excess reagent by rotary evaporation, the residual oil was purified by column chromatography on silica gel, using diethyl ether/methanol (9/1) as eluant. Compound 1 was obtained as an oil; 0.65 g (85%); IR (neat) 1725, 1650 cm-1 ; NMR (CDCl3) δ6.25 (s, 1H); 4.0 (t, 2H); 2.9 (t, 2H); 2.2 (s, 3H).

WORKUP

后处理

  1. temperatureAfter cooling
  2. customremoval of toluene and excess reagent
  3. customby rotary evaporation
  4. customthe residual oil was purified by column chromatography on silica gel