反应详情

To a mixture of lithium aluminium hydride (1.6 g) and dry tetrahydrofuran (10 ml), a solution of 3-n-butylamino-4-phenoxy-5-sulfamylbenzamide (2.25 g) in dry pyridine (20 ml) is added, and the mixture is refluxed for 16 hours. After cooling, ethyl acetate (1 ml) followed by water (6 ml) are very cautiously added dropwise, whereafter the mixture is stirred for a further 30 minutes. It is then heated on a steambath and filtered hot; the filter-cake is carefully washed with hot 2-methoxyethanol (3 portions of 20 ml). The combined filtrates are evaporated in vacuo and the residue is crystallized from ethanol to give 3-n-butylamino-4-phenoxy-5-sulfamylbenzylamine with a melting point of 195°-198° C.

1. temperaturethe mixture is refluxed for 16 hours
2. temperatureAfter cooling
3. additionare very cautiously added dropwise, whereafter the mixture
4. temperatureIt is then heated on a steambath
5. filtrationfiltered hot
6. washthe filter-cake is carefully washed with hot 2-methoxyethanol (3 portions of 20 ml)
7. customThe combined filtrates are evaporated in vacuo
8. customthe residue is crystallized from ethanol