反应详情

温度

0 °C

Bromine (136 mg, 0.85 mmol) was added to a-78° C. solution of triphenylphosphine (244 rag, 0.93 mmol) in 4 mL CH2Cl2, and the mixture was stirred 0.5 h at 0° C. and 5 rain at r.t. before recooling to -5° C. The alcohol from Step 8 (319 mg, 0.77 mmol) was then slowly added as a 1 mL CH2Cl2 solution and the mixture was stirred 2 h at 0° C. The reaction mixture was partitioned between CH2Cl2 and saturated NaHCO3. The organic layer was dried over MgSO4, concentrated and the residue purified by flash chromatography (10% ethyl acetate in hexane) to give 166 mg of the title compound.

1. customat r.t.
2. custombefore recooling to -5° C
3. stirringthe mixture was stirred 2 h at 0° C
4. customThe reaction mixture was partitioned between CH2Cl2 and saturated NaHCO3
5. dry with materialThe organic layer was dried over MgSO4
6. concentrationconcentrated
7. customthe residue purified by flash chromatography (10% ethyl acetate in hexane)