HRID260112

反应详情

EQUATION

反应方程式

HRID 260112 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of methyl (E) 6-(1,3-dihydro-7-methyl-3-oxo-4-p-toluenesulfonyloxy-6-vinyl isobenzofuran-5-yl)-4-methyl-4-hexenoate (0.37 g) and lithium hydroxide (0.4 g) in methanol (6 ml) and water (6 ml) was heated at 62° C. for 15 hours. The reaction was acidified with aqueous sodium hydrogen sulfate and extracted with ethyl acetate. The extract was dried and evaporated and the residue chromatographed on silica gel, eluting with ethyl acetate/hexane/acetic acid to give (E) 6-(1,3-dihydro-4-hydroxy-7-methyl-3-oxo-6-vinylisobenzofuran-5-yl)-4-methyl-4-hexenoic acid, m.p. 148° 149° C. (tert-butylmethyl ether/hexane).

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. customThe extract was dried
  3. customevaporated
  4. customthe residue chromatographed on silica gel
  5. washeluting with ethyl acetate/hexane/acetic acid