反应详情

To a 0° C. solution of the sulfide (19 g) from Step 4 in toluene (400 mL) was added Na2WO4.2H2O (0.16 g) and Bu4NHSO4 (0.81 g). Then 30% hydrogen peroxide (12.2 mL) was slowly added and the mixture was stirred at room temperature for 4.5 hours. The mixture was poured slowly on a mixture of ice, dilute aqueous sodium thiosulfate and ethyl acetate. The organic layer was separated and the aqueous further extracted with ethyl acetate (2×100 mL). The combined organic layers were washed with brine, dried with magnesium sulfate and the solvent were removed in vacuo to yield a residue which was purified purified on SiO2 using ethyl acetate and hexanes (1:1) as eluant to yield the product.

1. customThe organic layer was separated
2. extractionthe aqueous further extracted with ethyl acetate (2×100 mL)
3. washThe combined organic layers were washed with brine
4. dry with materialdried with magnesium sulfate
5. customthe solvent were removed in vacuo
6. customto yield a residue which
7. customwas purified
8. custompurified on SiO2
9. customto yield the product