HRID323887
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionare added
- customThe phases are separated
- extractionthe aqueous phase is extracted with 2×20 ml of 1,2-dichloroethane
- customthe combined organic layer is evaporated in vacuo
- customResidue: 22 g, fast crystallizing oil
- customThe raw product is recrystallized from 80 ml of isopropyl acetate