HRID22177

反应详情

EQUATION

反应方程式

HRID 22177 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.9 g of 7-hydroxy-3-methyl-phthalide (see Examples 101 and 111) and 5.1 g of Lawesson reagent are heated in 20 ml of xylene for 4 hours at 140° C. Chromatographic filtration of the mixture on silica gel (eluant: ethyl acetate/n-hexane (1:9)] yields 7-hydroxy-3-methylisobenzofuran-1(3H)-thione, m.p. 39°-41° C.; IR spectrum (CHCl3): C=O 1624, 1604, 1368, 1330, 1304, 1165 cm-1 ; mass spectrum: 180 (M+ =100), 165(58), 137(24).

WORKUP

后处理

  1. filtrationChromatographic filtration of the mixture on silica gel (eluant