反应详情

To a solution of (3-n-butylamino-4-phenoxy-5-sulfamylbenzyl)benzylamine (8.8 g; prepared as described in Example 136) in 2-methoxyethanol (90 ml), palladium (10%) on carbon (4.0 g) is added and the mixture is hydrogenated. After about 5 hours the theoretical amount of hydrogen has been absorbed, and the mixture is heated on a steam-bath and filtered to remove the catalyst. The filtrate is evaporated in vacuo and the residue triturated with water to yield crude 3-n-butylamino-4-phenoxy-5-sulfamylbenzylamine. The crude amine is dissolved in formic acid (50 ml), whereafter the solution is evaporated in vacuo. The residue is recrystallized from a mixture of ethanol and 2-methoxyethanol to yield, after filtration and drying, 3-n-butylamino-4-phenoxy-5-sulfamylbenzylamine formate hemihydrate with a melting point of 224°-226° C.

1. customAfter about 5 hours the theoretical amount of hydrogen has been absorbed
2. temperaturethe mixture is heated on a steam-bath
3. filtrationfiltered
4. customto remove the catalyst
5. customThe filtrate is evaporated in vacuo
6. customthe residue triturated with water