反应详情

To a solution of 3-azido-4-oxo-2,3,4,5-tetrahydro-1H-naphtho-[2,1-b]azepine (16.0 g, 63.4 mmol) in a mixture of dry dioxane (150 ml) and ethanol (150 ml), palladium on carbon (10%, 2 g) was added. This mixture was hydrogenated under a pressure of 5 bar and with efficient stirring for 24 h. The reaction mixture was filtered and excess hydrogenchloride in ethanol was added. The precipitated solid was isolated, washed with ethanol and dried to give 14.4 g of 3-amino-4-oxo-2,3,4,5-tetrahydro-1H-naphtho[2,1-b]azepine hydrochloride. The above hydrochloride (14.2 g) was dissolved into water (800 ml) by warming. A 25% aqueous ammonia solution was added and a precipitate was formed. The solid was isolated by filtration, washed with water and dried in vacuo to give 11.9 g of 3-amino-4-oxo-2,3,4,5-tetrahydro-1H-naphtho[2,1-b]azepine.

1. temperatureby warming
2. customa precipitate was formed
3. customThe solid was isolated by filtration
4. washwashed with water
5. customdried in vacuo