HRID465617

反应详情

EQUATION

反应方程式

HRID 465617 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 1.3 g (2.7 mmol) of ethyl 8-(p-chlorophenylsulfonamido)-4-[2-(3-pyridyloxy)ethyl]-octanoate in 8.1 ml acetonitrile is added 2.7 ml (5.4 mmol) 2M LiOH solution in water. After 18 h at room temperature, the reaction mixture is diluted with 9.5 ml water and filtered to remove a small amount of insoluble solid. The filtrate is acidified with 0.36 g (5.94 mmol) acetic acid and stirred in an ice bath. After 2 h the solid is filtered, washed with water and dried. Recrystallization from acetonitrile gives pure compound of example 31, namely 8-(p-chlorophenylsulfonamido)-4-[2-(3-pyridyloxy)ethyl)-octanoic acid, m.p. 86°-88°; further recrystallization gives m.p. 89°-91°. Compound forms potassium salt as hydrate (containing 1.5 moles water).

WORKUP

后处理

  1. filtrationfiltered
  2. customto remove a small amount of insoluble solid
  3. filtrationAfter 2 h the solid is filtered
  4. washwashed with water
  5. customdried
  6. customRecrystallization from acetonitrile