HRID1646966

反应详情

EQUATION

反应方程式

HRID 1646966 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 7.4 g of the product of Step A, 4.4 g of methyl methylsulfinyl methyl sulfide, 75 ml of tetrahydrofuran and 7 ml of Triton B was refluxed for one hour and then was poured into water and extracted with dichloromethane. The extracts were dried and concentrated to obtain 10 ml of produce which was dissolved in a 2N hydrochloric acid solution in methanol. The solution was stirred for 24 hours, treated with sodium bicarbonate, and stirred for one hour. After separating, extraction was carried out with ether and the extracts were washed and concentrated to obtain 9 g of product which was chromatographed on silica to obtain (eluant: hexane-ethyl acetate (9-1)) 4.3 g of the desired product which was used as is.

WORKUP

后处理

  1. temperaturewas refluxed for one hour
  2. extractionextracted with dichloromethane
  3. customThe extracts were dried
  4. concentrationconcentrated
  5. customto obtain 10 ml
  6. customof produce which
  7. stirringstirred for one hour
  8. customAfter separating
  9. extractionextraction
  10. washthe extracts were washed
  11. concentrationconcentrated