HRID465560

反应详情

EQUATION

反应方程式

HRID 465560 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 0.47 ml dimethylsulfoxide in 19 ml methylene chloride is cooled to -70° and 0.41 ml oxalyl chloride is added slowly. The solution is stirred at -70° for 15 min and a solution of 0.38 g of methyl 8-(p-chlorophenylsulfonamido)-4-(2-hydroxyethyl)-octanoate (example 28) in 1 ml methylene chloride is added slowly. The solution is stirred at -60° for 15 min and 1.9 ml triethylamine is added. The mixture is allowed to warm up to room temperature, washed with saturated sodium bicarbonate solution, and the organic phase is dried, filtered and evaporated to obtain a yellow oil. This oil is taken up in ether and washed with saturated sodium bicarbonate solution. The ether layer is dried, filtered and evaporated to yield methyl 8-(p-chlorophenylsulfonamido)-4-(formylmethyl)-octanoate.

WORKUP

后处理

  1. stirringThe solution is stirred at -60° for 15 min
  2. washwashed with saturated sodium bicarbonate solution
  3. customthe organic phase is dried
  4. filtrationfiltered
  5. customevaporated
  6. customto obtain a yellow oil
  7. washwashed with saturated sodium bicarbonate solution
  8. dry with materialThe ether layer is dried
  9. filtrationfiltered
  10. customevaporated