HRID342869

反应详情

EQUATION

反应方程式

HRID 342869 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Chlorosulphonic acid (1 molar equivalent) was added to a solution of the product from step (f) (15 g) in dichloroethane (90 ml) at a temperature of <16° C. When addition was complete, the mixture was stirred for 2 hours at room temperature and then evaporated in vacuo. Water (60 ml) and 5% w/v aqu. NaOH (41 ml) were added and the mixture distilled at atmospheric pressure. The organic phase of the distillate was separated and dried over KOH to give a solution of the desired product (77% yield).

WORKUP

后处理

  1. additionWhen addition
  2. customevaporated in vacuo
  3. additionNaOH (41 ml) were added
  4. distillationthe mixture distilled at atmospheric pressure
  5. customThe organic phase of the distillate was separated
  6. dry with materialdried over KOH