反应详情

温度

2.5 °C

The title compound of step 1 (70.8 g, 261 mmol) in a mixture of acetic acid (810 mL) and concentrated hydrochloric acid (354 mL) was heated to boiling for 3.5 h under DC control. The mixture was then cooled to 0 to 5° C., diluted with water (1 L), saturated with NaCl and extracted cold with ethyl acetate (3×300 mL). The ethyl acetate phase was washed with water and concentrated to low volume in a vacuum. The solid residue was dissolved once again in ethyl acetate, washed with NaHCO3 solution and concentrated until dry.

1. temperaturewas heated
2. extractionextracted cold with ethyl acetate (3×300 mL)
3. washThe ethyl acetate phase was washed with water
4. concentrationconcentrated to low volume in a vacuum
5. dissolutionThe solid residue was dissolved once again in ethyl acetate
6. washwashed with NaHCO3 solution
7. concentrationconcentrated
8. customuntil dry