反应详情

The product from Example 66A (10.0 g, 64 mmol) in methanol (320 mL) was treated with mercury(II) acetate (2.0 g, 6.4 mmol) and sulfuric acid (0.5 mL). After refluxing for 1.5 hours, the mixture was allowed to cool to ambient temperature, concentrated to a volume of 100 mL, poured into 1N HCl (300 mL) and extracted with dichloromethane (3×300 mL). The organic layers were combined, washed with aqueous NaHCO3, washed with brine, dried over Na2SO4 and concentrated to provide the title compound (10.3 g).

1. temperatureAfter refluxing for 1.5 hours
2. concentrationconcentrated to a volume of 100 mL
3. additionpoured into 1N HCl (300 mL)
4. extractionextracted with dichloromethane (3×300 mL)
5. washwashed with aqueous NaHCO3
6. washwashed with brine
7. dry with materialdried over Na2SO4
8. concentrationconcentrated