反应详情

温度

0 °C

To a 0° C. suspension of lithium aluminum hydride (4 eq) in dry THF (250 mL) was added portionwise phtalic anhydride over 20 minutes. The mixture was brought to room temperature then warmed to reflux for 6 hours then cooled to 0° C. The reaction was quenched with saturated sodium sulfate solution, filtered and concentrated. The residue was taken into ethyl acetate washed with water, brine, dried and concentrated to yield the desired compound as a viscous oil. 1HNMR (500 mHz, CDCl3): 5.62 ppm (s, 2H); 3.76-3.70 (m, 2H); 3.72-3.55 (m, 4H), 2.20-1.98 (m, 6H).

1. customwas brought to room temperature
2. temperaturethen warmed
3. temperatureto reflux for 6 hours
4. customThe reaction was quenched with saturated sodium sulfate solution
5. filtrationfiltered
6. concentrationconcentrated
7. washwashed with water, brine
8. customdried
9. concentrationconcentrated