反应详情

温度

-30 °C

The compound of step 1 (100 mg, 0.327 mmol) was dissolved in THF (1.5 ml) and the mixture was cooled to −30° C. Phenyl chloroformate (77.6 mg, 0.49 mmol) was added and the mixture was stirred for 10 minutes. Ethyl magnesiumbromide (0.589 ml, 1M in THF) was added at −30° C. and the mixture was stirred for 30 minutes, partitioned between diethylether and aqueous ammonium chloride solution, the combined organic extracts were dried over sodium chloride and evaporated to dryness in vacuo. The raw material was purified by silica gel chromatography with a heptane/ethyl acetate gradient to yield the title compound (84 mg).

1. stirringthe mixture was stirred for 30 minutes
2. custompartitioned between diethylether and aqueous ammonium chloride solution
3. dry with materialthe combined organic extracts were dried over sodium chloride
4. customevaporated to dryness in vacuo
5. customThe raw material was purified by silica gel chromatography with a heptane/ethyl acetate gradient