反应详情

温度

60 °C

InBr3 (0.056 mmol) and Et3SiH (12.6 mmol) were successively added to a solution of lactone 16A (0.54 mmol) in CHCl3 (5 mL) and the reaction mixture was heated at 60° C. for 1 h. The reaction mixture was allowed to cool to rt, was diluted with H2O (10 mL), and the layers were separated. The aqueous layer was extracted with DCM (3×10 mL) and the combined organic layers were dried (Na2SO4) and concentrated. The residue was purified by silica gel chromatography (10/90 to 30/70 EtOAc/hexane) to provide ether 16B in 70% yield. Data: LC/MS (ESR) m/z 210 [M+1]+.

1. temperatureto cool to rt
2. customthe layers were separated
3. extractionThe aqueous layer was extracted with DCM (3×10 mL)
4. dry with materialthe combined organic layers were dried (Na2SO4)
5. concentrationconcentrated
6. customThe residue was purified by silica gel chromatography (10/90 to 30/70 EtOAc/hexane)