反应详情

温度

80 °C

Methyl 3-(1-hydroxyphthalazin-6-yl)-4-methylbenzoate (2.85 g, 9.68 mmol) was suspended in acetonitrile (19.4 mL), cooled to 0° C. to which phosphorus oxychloride (1.81 mL, 19.4 mmol) was added dropwise. The reaction mixture was warmed to 80° C. for 2.5 h, then concentrated, diluted with 150 mL of ethyl acetate, added to a separatory funnel and partitioned with water. The organics were washed 2×50 mL with water, separated, dried over sodium sulfate, and concentrated in vacuo to give the title compound. MS (ES+): 313(M+H)+.

1. additionwas added dropwise
2. concentrationconcentrated
3. additiondiluted with 150 mL of ethyl acetate
4. additionadded to a separatory funnel
5. custompartitioned with water
6. washThe organics were washed 2×50 mL with water
7. customseparated
8. dry with materialdried over sodium sulfate
9. concentrationconcentrated in vacuo