反应详情

温度

0 °C

2-methyl-2-phenyl-propanol (Intermediate 3) (0.5 kg) and pyridine (268 ml) were charged to a reactor and chilled to 0° C. Acetic anhydride (680 gms) was slowly added through a dropper at 10-20° C. The mixture was stirred for 2 hours at 10-20° C. Ethyl acetate (1.5 ltr) was added and chilled water (2 ltrs) was slowly added through a dropper at 10-20° C. The mixture was stirred for ½ hr. The ethyl acetate layer was separated and 10% chilled dilute HCl was added. The ethyl acetate layer was then washed with sodium bicarbonate until a pH of 7 was obtained. The ethyl acetate layer was dried with sodium sulphate and concentrated under vacuum. The resulting oil was distilled under vacuum (15 mm of Hg), at 80-100° C.

1. additionwas slowly added through a dropper at 10-20° C
2. stirringThe mixture was stirred for ½ hr
3. customThe ethyl acetate layer was separated
4. temperature10% chilled dilute HCl
5. additionwas added
6. washThe ethyl acetate layer was then washed with sodium bicarbonate until a pH of 7
7. customwas obtained
8. dry with materialThe ethyl acetate layer was dried with sodium sulphate
9. concentrationconcentrated under vacuum
10. distillationThe resulting oil was distilled under vacuum (15 mm of Hg), at 80-100° C.