反应详情

温度

70 °C

To a solution of 17-ethyl-1-hydroxy-12-[2'-(4"-azido-3"-propyloxycyclohexyl)-1'-methylvinyl]-23,25-dimethoxy-13,19,21,27-tetramethyl-11,28-dioxa-4-azatricyclo[22.3.1.04,9 ]octacos-18-ene-2,3,10,16-tetraone (46 mg) in 10% aqueous benzene (900 μl) was added triphenylphosphine (29 mg) and the mixture heated to 70° C. with stirring. After 6.5 hours, the stir bar was removed and the reaction cooled to room temperature. The mixture was concentrated to 10% volume in vacuo and applied directly to a column of silica gel for purification by flash chromatography (ethyl acetate: hexane (1:1)+1% methanol then 2% ammonium hydroxide, 5% methanol in methylene chloride) to give the title compound (37 mg).

1. customthe stir bar was removed
2. temperaturethe reaction cooled to room temperature
3. concentrationThe mixture was concentrated to 10% volume in vacuo
4. customapplied directly to a column of silica gel for purification by flash chromatography (ethyl acetate: hexane (1:1)+1% methanol