HRID1494149
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
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 for 48 hours. 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
- additionis added
- customThe precipitated product is collected
- stirringThe suspension is stirred
- customthe precipitate is collected
- washwashed with water
- customdried at 60°/3 mm Hg for 48 hours
- customThe product is recrystallized twice from ethyl acetate and once from acetonitrile