HRID613987

反应详情

EQUATION

反应方程式

HRID 613987 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

4,5-Dimethyl-2-methylthiooxazole (4.21 g, 0.029 m) in dry chloroform (15 ml) was cooled to 0° C. and anhydrous sodium carbonate (8.0 g, 0.0755 m) added. 88.5% 3-Chloroperbenzoic acid (11.5 g, 0.059 m) in dry chloroform was then added over 45 minutes, and the mixture stirred for a further 45 minutes at 0° C. Solid sodium sulphite (5 g) was then added and the mixture allowed to warm to room temperature. The mixture was then filtered and the filtrate evaporated, the residue being chromatographed on silica using diethyl ether. The resulting solid was recrystallised from ethyl acetate/hexane as the title product, m.p. 42° C.

WORKUP

后处理

  1. temperatureto warm to room temperature
  2. filtrationThe mixture was then filtered
  3. customthe filtrate evaporated
  4. customthe residue being chromatographed on silica
  5. customThe resulting solid was recrystallised from ethyl acetate/hexane as the title product, m.p. 42° C.