反应详情

To a solution of 4A (1 g) in toluene (10 ml) is added a 2 M solution of potassium carbonate in water (2.5 ml) under an inert gas atmosphere. A suspension of 4B (0.66 g) and tetrakis(triphenylphosphine)palladium (0.15 g) in methanol (3 ml) is added and the mixture is heated to for 36 h to reflux. After cooling, the organic phase is separated and the water phase is washed twice with ethyl acetate. The combined organic phases are dried, evaporated to dryness and the residue is purified by silica-gel flash chromatography and preparative HPLC. One obtains the title compound as colorless crystals of mp. 113° C.

1. additionis added
2. temperaturethe mixture is heated to for 36 h
3. temperatureto reflux
4. temperatureAfter cooling
5. customthe organic phase is separated
6. washthe water phase is washed twice with ethyl acetate
7. customThe combined organic phases are dried
8. customevaporated to dryness
9. customthe residue is purified by silica-gel flash chromatography and preparative HPLC