反应详情

A degassed solution of 3-amino-1H-pyrrolo[3,2-c]pyridine-2-carboxylic acid ethyl ester (200 mg, 0.98 mmol), trifluoro-methanesulfonic acid 2-fluoro-4-trimethylsilanyl-phenyl ester (324 mg, 1.02 mmol), Pd2dba3 (44 mg, 0.048 mmol), Xantphos (56 mg, 0.098 mmol) and Cs2CO3 (636 mg, 1.95 mmol) in toluene (6 ml) was subjected to microwave irradiation at 150° C. for 20 minutes. The reaction mixture was cooled to ambient temperature then diluted with EtOAc (100 ml). The resultant solution was washed with water (60 ml), dried (Na2SO4) and concentrated in vacuo to give a black oil. The oil was purified by flash chromatography (Si-PPC, cyclohexane:EtOAc, gradient 90:10 to 20:80) to provide the title compound as a brown solid (152 mg, 42%). LCMS (method B): RT=2.65 min, M+H+=372.

1. customirradiation at 150° C. for 20 minutes
2. washThe resultant solution was washed with water (60 ml)
3. dry with materialdried (Na2SO4)
4. concentrationconcentrated in vacuo
5. customto give a black oil
6. customThe oil was purified by flash chromatography (Si-PPC, cyclohexane:EtOAc, gradient 90:10 to 20:80)