反应详情

温度

50 °C

To a solution of 0.13 g (0.38 mmol) of ethyl 4-[(5,6,7,8-tetrahydro-5-hydroxy-8,8-dimethylnaphth-2-yl)ethynyl]benzoate (Compound 9) in 15 ml of dry benzene was added 0.67 g (2.90 mmol) of (methoxycarbonylsulfamoyl) triethylammonium hydroxide (Burgess Reagent). The resulting mixture was heated at 50° C. for 30 minutes, cooled to room temperature, partitioned between water (10 ml) and EtOAc (20 ml) and the layers separated. The organic layer was dried over Na2SO4, concentrated in vacuo and purified by flash chromatography (silica, 10% EtOAc-hexane) to yield the title compound as a clear oil.

1. temperaturecooled to room temperature
2. custompartitioned between water (10 ml) and EtOAc (20 ml)
3. customthe layers separated
4. dry with materialThe organic layer was dried over Na2SO4
5. concentrationconcentrated in vacuo
6. custompurified by flash chromatography (silica, 10% EtOAc-hexane)