反应详情

40 mg (0.09 mmol) of the compound from example 7 are absorbed in 1 ml acetone and mixed with 1 ml water, 74 mg (0.29 mmol) magnesium nitrate hexahydrate and 32 mg (0.20 mmol) potassium permanganate. The reaction mixture is stirred for 24 hours at room temperature, diluted with 5 ml acetonitrile and filtered through a Millipore filter. The filtrate is extracted twice with dichloromethane and the combined organic phases washed with a saturated sodium chloride solution, dried using sodium sulfate, filtered and evaporated under vacuum until dryness. The residue is recrystallized from acetonitrile. This produces 14 mg (25% of theoretical yield, 75% purity) of the title compound.

1. filtrationfiltered through a Millipore
2. filtrationfilter
3. extractionThe filtrate is extracted twice with dichloromethane
4. washthe combined organic phases washed with a saturated sodium chloride solution
5. customdried
6. filtrationfiltered
7. customevaporated under vacuum until dryness
8. customThe residue is recrystallized from acetonitrile