反应详情

To a stirred solution of 1-4 (0.10 g, 0.39 mmol), Pd(OAc)2 (0.004 g, 0.02 mmol), xphos (0.02 g, 0.039 mmol) in dioxane (3 mL) was added 3-ethoxy-3-oxopropylzinc bromide 0.5M solution in THF (3.15 mL, 1.57 mmol) and the resulting mixture was microwave irradiated for 30 minutes at 100° C. The reaction was allowed to cool and partitioned between ethyl acetate and water. The organic phase was concentrated and flash column separation using a 0-30% ethyl acetate/hexane gradient gave 37-1. (0.10 g, 86%). LRMS (ES) (M+H)+: observed=320.1, calculated=320.4.

1. customthe resulting mixture was microwave irradiated for 30 minutes at 100° C
2. temperatureto cool
3. custompartitioned between ethyl acetate and water
4. concentrationThe organic phase was concentrated
5. customflash column separation
6. customgave 37-1