反应详情

A solution of 25.2 g. of 3-fluoro-4-(hexadecylamino)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 HCl, and the organic layer separated, dried (MgSO4), and evaporated. Crystallization of the residual white solid from 60% aqueous acetic acid and then from methylene chloridehexane affords N-[3-fluoro-4-(hexadecylamino)benzoyl]methanesulfonamide as a white solid.

1. temperatureunder reflux for 2 hours
2. concentrationconcentrated in vacuo
3. customThe residue is partitioned between water and diethyl ether
4. customthe organic layer separated
5. dry with materialdried (MgSO4)
6. customevaporated
7. customCrystallization of the residual white solid from 60% aqueous acetic acid