HRID568125

反应详情

EQUATION

反应方程式

HRID 568125 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

24.8 g (0.075 mol) of [2-(2-thienyl)ethylamino](2-chlorophenyl)acetamide hydrochloride, prepared according to example 5 or 6, is mixed with 170 ml of water, then under mild cooling 30 ml of 10% sodium hydroxide solution and 170 ml of 1,2-dichloroethane are added. The phases are separated, the aqueous phase is extracted with 2×20 ml of 1,2-dichloroethane, the combined organic layer is evaporated in vacuo. Residue: 22 g, fast crystallizing oil. The raw product is recrystallized from 80 ml of isopropyl acetate to give 19.5 g of the crystalline base of formula (VII). Yield: 88.2%, mp.: 90-92° C.

WORKUP

后处理

  1. additionare added
  2. customThe phases are separated
  3. extractionthe aqueous phase is extracted with 2×20 ml of 1,2-dichloroethane
  4. customthe combined organic layer is evaporated in vacuo
  5. customResidue: 22 g, fast crystallizing oil
  6. customThe raw product is recrystallized from 80 ml of isopropyl acetate