反应详情

Hydrazine hydrate (4.65 ml, 0.09 mole) was added to a solution of methyl 3-[2-(2-hydroxy-3-isopropylaminopropoxy) benzoyl]propionate (10 g, 0.03 mole) in glacial acetic acid (80 ml) and the solution was heated under reflux for one hour. Evaporation under reduced pressure gave an oil (25.5 g.) which was dissolved in water, treated with an excess of sodium carbonate solution and extracted with dichloromethane. Evaporation of the dried extracts gave an oil (10.3 g.) which was purified on a silica column by elution with a mixture of chloroform and methanol to give 6-[2-(2-hydroxy-3-isopropyl-aminopropoxy)-phenyl]-4,5-dihydro-3(2H)-pyridazinone (6.25 g, 66%), m.p. 124°-126° C. The hydrochloride, crystallised from 2-propanol, had m.p. 162°-164.5° C.

1. temperaturethe solution was heated
2. temperatureunder reflux for one hour
3. customEvaporation under reduced pressure
4. customgave an oil (25.5 g.) which
5. extractionextracted with dichloromethane
6. customEvaporation of the dried extracts
7. customgave an oil (10.3 g.) which
8. customwas purified on a silica column by elution with a mixture of chloroform and methanol