HRID1109612
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureAfter cooling
- customremoval of toluene and excess reagent
- customby rotary evaporation
- customthe residual oil was purified by column chromatography on silica gel