反应详情

温度

90 °C

Ethyl 3-(1-hydroxyphthalazin-6-yl)-4-methylbenzoate (5.5 g) was suspended in acetonitrile (50 mL), and was treated with phosphorus oxychioride (3 mL, 36 mmol). The mixture was stirred at 90° C. for 4 h. The mixture was concentrated to remove all solvent, and redissolved in ethyl acetate (200 mL). The organic solution was washed with water (3×20 mL), brine (20 mL), and was dried over anhydrous Na2SO4, and concentrated in vacuo to give ethyl 3-(1-chlorophthalazin-6-yl)-4-methylbenzoate as a pale yellow solid.

1. concentrationThe mixture was concentrated
2. customto remove all solvent
3. dissolutionredissolved in ethyl acetate (200 mL)
4. washThe organic solution was washed with water (3×20 mL), brine (20 mL)
5. dry with materialwas dried over anhydrous Na2SO4
6. concentrationconcentrated in vacuo