反应详情

A solution of the product of stage (iv) (3.2 g) in THF (50 ml) was added to a stirred suspension of mercury (II) chloride (8.5 g) and calcium carbonate (3.2 g) in methanol-water (9:1, 50 ml) and the mixture was stirred at reflux for 1 h. The reaction was filtered through hyflo, the filtrate was concentrated in vacuo and the resulting oil was dissolved in chloroform (50 ml). The resulting precipitate was removed by filtration, the solvent was evaporated and the residue was purified by FCC (System D 19:1→4:1) to give the title compound as a crystalline mass (1.4 g) m.p. 30°-31°.

1. temperatureat reflux for 1 h
2. filtrationThe reaction was filtered through hyflo
3. concentrationthe filtrate was concentrated in vacuo
4. dissolutionthe resulting oil was dissolved in chloroform (50 ml)
5. customThe resulting precipitate was removed by filtration
6. customthe solvent was evaporated
7. customthe residue was purified by FCC (System D 19:1→4:1)