反应详情

温度

23 °C

Combine a solution of the product of Step 2 (13.2 g, 65 mmol) in CH2 Cl2 (250 mL) at 0° C. with pyridine (7.89 mL, 97.5 mmol) and dimethylaminopyridine (DMAP) (397 mg, 3.25 mmol), followed by acetyl chloride (6.48 mL, 74.7 mmol). Allow the mixture to warm to 23° C., pour into 1M HCl (100 mL) and wash the resulting organic layer with 1M HCl (100 mL) followed by water (5×100 mL; pH=6.5-7). Dry the organic layer over Na2SO4 and concentrate, providing 3-(3,4-dichloro-phenyl)-2-propene-1-ol acetate as a colorless oil, 15.4 g (62.9 mmol, 97%).

1. customat 0° C.
2. washwash the resulting organic layer with 1M HCl (100 mL)
3. dry with materialDry the organic layer over Na2SO4
4. concentrationconcentrate