反应详情

A solution of the product of example 3 step (vii) (2.5 g) in dry dimethylsulphoxide (30 ml) was treated with cesium carbonate (10 g) with stirring. After 20 min a solution of the product of step (ii) (1.5 g) in dimethylsulphoxide (10 ml) was added dropwise over 2 min. After 1.5 hours the reaction mixture was quenched with saturated brine and the product extracted into ethyl acetate. The organic phase was dried (MgSO4) and the solvent was evaporated under reduced pressure to leave a brown gum. Column chromatography eluting with 10% methanol in ethyl acetate containing 1% triethylamine gave the product as a glass.

1. customAfter 1.5 hours the reaction mixture was quenched with saturated brine
2. extractionthe product extracted into ethyl acetate
3. dry with materialThe organic phase was dried (MgSO4)
4. customthe solvent was evaporated under reduced pressure
5. customto leave a brown gum
6. washColumn chromatography eluting with 10% methanol in ethyl acetate containing 1% triethylamine