反应详情

3.7 ml diethyl dithiophosphate was added to a mixture of 2.0 g 4-[(3-chloro-4-methoxybenzyl)amino]-1-(hydroxypiperidino)-6-phthalazine carbonitrile, 1 ml water and 2 ml isopropanol, and the mixture was heated under reflux for 1 hr. After cooling, water was added to the reaction solution and the resulting crystals were collected by filtration. The filtrate was extracted with ethyl acetate and washed with brine. It was dried over anhydrous sodium sulfate, and filtered. The filtrate was evaporated, and the resulting crystalline residue was combined with the crystals collected above by filtration, whereby 1.5 g of the title compound was obtained.

1. temperaturethe mixture was heated
2. temperatureunder reflux for 1 hr
3. temperatureAfter cooling
4. filtrationthe resulting crystals were collected by filtration
5. extractionThe filtrate was extracted with ethyl acetate
6. washwashed with brine
7. dry with materialIt was dried over anhydrous sodium sulfate
8. filtrationfiltered
9. customThe filtrate was evaporated
10. filtrationcollected above by filtration