反应详情

The above intermediate 5-hydrazino-1,6-naphthyridin-2(1H)-one as its monohydrochloride monohydrate was prepared as follows. A mixture containing 30 g of 5-bromo-1,6-naphthyridin-2(1H)-one and 20.2 ml of hydrazine hydrate was heated to reflux and then heated for an additional 2 hours. The reaction mixture was concentrated on a rotary evaporator and the residue was slurried in concentrated hydrochloric acid. The solid was collected, washed with concentrated hydrochloric acid, dried in a vacuum oven at 75° C. The solid was then slurried in water, collected by filtration, washed with water and dried in a vacuum oven at 90° C. to yield 25.2 g of 5-hydrazino-1,6-naphthyridin-2(1H)-one monohydrochloride monohydrate, m.p. >310° C. with decomposition.

1. temperaturewas heated
2. temperatureto reflux
3. temperatureheated for an additional 2 hours
4. concentrationThe reaction mixture was concentrated on a rotary evaporator
5. customThe solid was collected
6. washwashed with concentrated hydrochloric acid
7. customdried in a vacuum oven at 75° C
8. filtrationcollected by filtration
9. washwashed with water
10. customdried in a vacuum oven at 90° C.