反应详情

To a solution of 17.1 g (0.053 mole) of sulfamic acid 2-[3-(phenylmethoxy)phenoxy]ethyl ester in 250 ml of tetrahydrofuran was added 0.5 teaspoon of 5% palladium on carbon catalyst and the mixture was hydrogenated in a Parr bottle at 40° C. for 2 hr. The catalyst was removed and a fresh 0.5 teaspoon of 5% palladium on carbon catalyst was added and the mixture was hydrogenated at 40° C. for 19 hr, whereby hydrogen uptake ceased. The catalyst was removed by filtration through Celite® and the solvent was evaporated under reduced pressure to yield 12.3 g of a brown, viscous oil that solidified after standing for five weeks at ambient temperature. The solid was triturated with ethyl ether-petroleum ether into a paste. The solvents were decanted and the paste was dried to yield 8.9 g (72%) a white solid, mp 56°-60° C.

1. customThe catalyst was removed
2. additiona fresh 0.5 teaspoon of 5% palladium on carbon catalyst was added
3. waitthe mixture was hydrogenated at 40° C. for 19 hr
4. customThe catalyst was removed by filtration through Celite®
5. customthe solvent was evaporated under reduced pressure
6. customto yield 12.3 g of a brown, viscous oil that solidified
7. waitafter standing for five weeks at ambient temperature
8. customThe solid was triturated with ethyl ether-petroleum ether into a paste
9. customThe solvents were decanted
10. customthe paste was dried