反应详情

Concentrated sulfuric acid (40 ml) was added to a stirred solution of 1-Bromo-4-oxo-3,4-dihydro-phthalazine-6-carboxylic acid (85 g, 0.32 mol) in ethanol (500 ml) and the mixture was heated to reflux for 48 hours. After this time, the reaction mixture was cooled and the resulting precipitate was filtered. The precipitate was partitioned between ethyl acetate (1 L) and saturated NaHCO3 (500 ml), the organic layer was separated and washed with water (500 ml) before being dried (MgSO4), filtered and concentrated under vacuum to give the title compound (30 g, 31% yield) as a white solid. MS (ESI+)=(M+H)+ 297 & 299

1. temperaturethe mixture was heated
2. temperatureto reflux for 48 hours
3. temperatureAfter this time, the reaction mixture was cooled
4. filtrationthe resulting precipitate was filtered
5. customThe precipitate was partitioned between ethyl acetate (1 L) and saturated NaHCO3 (500 ml)
6. customthe organic layer was separated
7. washwashed with water (500 ml)
8. dry with materialbefore being dried (MgSO4)
9. filtrationfiltered
10. concentrationconcentrated under vacuum