HRID37425

反应详情

EQUATION

反应方程式

HRID 37425 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.20 g of ethyl p-(2,3,4,5-tetrahydro-1-benzothiepine-8-carboxamido)benzoate were dissolved in 40 ml of ethanol and treated with 14 ml of water containing 1.40 g of NaOH. The mixture was stirred at room temperature overnight, poured on to ice and acidified with conc. HCl. The mixture was then extracted twice with ethyl acetate, washed with water, dried and evaporated. Recrystallization from ethyl acetate gave 925 mg of p-(2,3,4,5-tetrahydro-1-benzothiepine-8-carboxamido)benzoic acid as colorless crystals of m.p. 261°-262° C.

WORKUP

后处理

  1. additionpoured on to ice
  2. extractionThe mixture was then extracted twice with ethyl acetate
  3. washwashed with water
  4. customdried
  5. customevaporated
  6. customRecrystallization from ethyl acetate