HRID1657552

反应详情

EQUATION

反应方程式

HRID 1657552 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of the sulfinic acid salt (26.0 g.) and 1-chloro-2-methyl-4-acetoxy-but-2-ene (9.75 g.) in 125 ml. of dimethylformamide was heated to 60°C. for 33/4 hours, cooled, poured into 1.21. of water and extracted with ethyl acetate. The extracts were washed with water and brine and dried. Removal of the solvent afforded 18.72 g. of the desired product. Chromatography of a 3.5 g. portion on silica gel gave 3.25 g. of the 1-(p-trifluoromethylphenylsulfonyl)-2-methyl-4-acetoxy-but-2-ene as a colorless oil. Anal. calcd. for C14H15F3O4S: C 50.00, H 4.50, S 9.53; found C 49.77, H 4.68, S 9.71%.

WORKUP

后处理

  1. temperaturecooled
  2. additionpoured into 1.21
  3. extractionof water and extracted with ethyl acetate
  4. washThe extracts were washed with water and brine
  5. customdried
  6. customRemoval of the solvent
  7. customafforded 18.72 g