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温度

0 °C

To the aldehyde of Step 10 (85 g, 386 mmol) in toluene (1 L) at 0° C. was slowly added vinyl magnesium bromide in Et2O (450 mL, 1M, 450 mmol) over a 30 minute period. After stirring for 1 hr at 0° C., the reaction mixture was quenched with 25% aq. NH4OAc and extracted with EtOAc (3×). Evaporation and purification by flash chromatography (15%→25% EtOAc in toluene) yielded 82 g (86%) of the title compound.

1. customat 0° C.
2. customover a 30 minute
3. customthe reaction mixture was quenched with 25% aq. NH4OAc
4. extractionextracted with EtOAc (3×)
5. customEvaporation and purification by flash chromatography (15%→25% EtOAc in toluene)