反应详情

To a solution of 17-ethyl-1,14-dihydroxy-12-[2'-(4"-(tert-butyldimethylsiloxy)-3"-allyloxycyclohexyl)-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 (150 mg) in acetonitrile (3 ml) was added a solution of 2% HF in aqueous acetonitrile (80 μl), and the mixture was stirred at room temperature. After 2 hours, the solution was diluted with ethyl acetate and quenched with saturated sodium bicarbonate. The layers were separated, and the organic layer was washed with brine and dried over magnesium sulfate. Purification of the concentrate by flash chromatography on silica gel (ethyl acetate:hexane (1:1)+1% methanol) gave the title compound (63 mg). 1H NMR consistent with the desired structure.

1. customquenched with saturated sodium bicarbonate
2. customThe layers were separated
3. washthe organic layer was washed with brine
4. dry with materialdried over magnesium sulfate
5. customPurification of the
6. concentrationconcentrate by flash chromatography on silica gel (ethyl acetate:hexane (1:1)+1% methanol)