HRID2291047

反应详情

EQUATION

反应方程式

HRID 2291047 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Similar procedures employed in Preparation J in reacting 3-(p-methylphenylsulfonyloxy)thiolane with potassium thioacetate by reacting 4-(p-methylphenylsulfonyloxy)thiane and 1.5 equivalents of potassium thioacetate at 80° C. in dimethylformamide to obtain 4-methylcarbonylthiothiane in 69% yield after chromatography on silica gel eluted with 10% ethyl acetate/hexane. The NMR spectrum of a deuterochloroform solution of 4-methylcarbonylthiothiane had peaks at 1.62-2.2 (4H, m); 2.32 (3H, s); 2.5-2.8 (4H, m); and 3.52 (1H, tt, J=9, 3 Hz) ppm.

WORKUP

后处理

  1. customSimilar procedures employed in Preparation J
  2. customat 80° C.