反应详情

Hydrogen sulphide was passed through a suspension of potassium tert-butoxide (9.31 g) in N,N-dimethylformamide (80 ml) at 5° C. until the mixture was saturated. The product from example 1 step (v) (5.0 g) was added and the reaction mixture stirred at room temperature for 2 h. The mixture was poured onto ice, acidified to pH3 and extracted with ethyl acetate. The organic phase was washed with water, dried (MgSO4) and evaporated under reduced pressure. Purification was by chromatography eluting with 40-50% ethyl acetate in isohexane.

1. additionThe mixture was poured onto ice
2. extractionextracted with ethyl acetate
3. washThe organic phase was washed with water
4. dry with materialdried (MgSO4)
5. customevaporated under reduced pressure
6. customPurification
7. washeluting with 40-50% ethyl acetate in isohexane