HRID465610

反应详情

EQUATION

反应方程式

HRID 465610 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3046 g of methyl 8-(p-chlorophenylsulfonamido)-4-[3-(3-pyridyl)propyl]-octanoate, 10 l of acetonitrile and 6701 ml of 2M lithium hydroxide is stirred at room temperature overnight, and then diluted with 20 l of water. Acetic acid (1 l) is added to adjust pH to 5.5 and additional water (12 l) is added. The precipitated product is collected and resuspended in 50 l of water. The suspension is stirred, the precipitate is collected, washed with water and dried at 60°/3 mm Hg (=4.00 mbar) for 48 h. The product is recrystallized twice from ethyl acetate and once from acetonitrile to yield 8-(p-chlorophenylsulfonamido)-4-[3-(3-pyridyl)propyl]-octanoic acid, m.p. 116.5°-118°.

WORKUP

后处理

  1. additionis added
  2. customThe precipitated product is collected
  3. stirringThe suspension is stirred
  4. customthe precipitate is collected
  5. washwashed with water
  6. customdried at 60°/3 mm Hg (=4.00 mbar) for 48 h
  7. customThe product is recrystallized twice from ethyl acetate and once from acetonitrile