HRID1105908
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 solution of 25.2 g. of 4-[15-(trifluoromethyl)pentadecylamino]benzoyl chloride hydrochloride and 5.6 g. of methanesulfonamide in 250 ml. of pyridine is stirred under reflux for 2 hours and then concentrated in vacuo. The residue is partitioned between water and diethyl ether; the aqueous layer acidified with 1 N hydrochloric acid, and the organic layer separated, dried over magnesium sulfate and evaporated. Crystallization of the residual white solid from 60% aqueous acetic acid and then from methylene chloride-hexane affords the product as a white solid.
WORKUP
后处理
- temperatureunder reflux for 2 hours
- concentrationconcentrated in vacuo
- customThe residue is partitioned between water and diethyl ether
- customthe organic layer separated
- dry with materialdried over magnesium sulfate
- customevaporated
- customCrystallization of the residual white solid from 60% aqueous acetic acid