反应详情

A solution of ethyl-3-hydroxymethyl-4-oxo-3-H-phthalazin-1-ylacetate (13.1 g), phosphorous tribromide (13.5 g) and anhydrous ether (250 ml) was stirred overnight at room temperature. It was then poured onto water (200 ml). The organic layer was collected, washed again with water (3×100 ml) and then dried over anhydrous sodium sulfate. The dried organic extract was evaporated to dryness and the resulting crude solid was purified by chromatography on silica gel, eluting with 95% CH2Cl2 -5% ethyl acetate (percents by volume) to obtain the title compound (yield: 9.8 g; m.p. 96° C.).

1. additionIt was then poured onto water (200 ml)
2. customThe organic layer was collected
3. washwashed again with water (3×100 ml)
4. dry with materialdried over anhydrous sodium sulfate
5. extractionThe dried organic extract
6. customwas evaporated to dryness
7. customthe resulting crude solid was purified by chromatography on silica gel
8. washeluting with 95% CH2Cl2 -5% ethyl acetate (percents by volume)