反应详情

A buffer was prepared by dissolving K2CO3 (20.7 g) and EDTA-Na2 (11.5 mg) in water (100 mL). 1,2-Dimethyl-3-(2-propenyl)benzene, compound of formula (XXIII), prepared according to example 3 (0.90 g, 6.16 mmol), was dissolved in a mixture of dichloromethane and acetonitrile (v/v 1:1, 60 mL), and the buffer prepared as described above (9.3 mL) was added. To the resulting mixture, first 1,1,1-trifluoroacetone (60 μL) and then hydrogen peroxide (30% in water, 6.2 mL, 60.7 mmol) were added and the mixture was stirred at room temperature for 2 h. The reaction mixture was diluted with water (100 mL), the organic phase was separated, and the aqueous phase was extracted with dichloromethane (2 times with 50 mL each). The combined organic phases were dried over Na2SO4, concentrated under reduced pressure, and the residue was purified by via silica gel column chromatography using hexane:ethyl acetate as eluent (v/v 32:1) to give 851 mg (85%) of the title compound.

1. customA buffer was prepared
2. customthe buffer prepared
3. additionwas added
4. customthe organic phase was separated
5. extractionthe aqueous phase was extracted with dichloromethane (2 times with 50 mL each)
6. dry with materialThe combined organic phases were dried over Na2SO4
7. concentrationconcentrated under reduced pressure
8. customthe residue was purified by via silica gel column chromatography