反应详情

Tetra-n-butylammoniumfluoride (1 mol/l tetrahydrofuran solution) 2.2 ml was added to compound (45) 496 mg in tetrahydrofuran 10 ml with cooling in ice. The mixture was stirred for 3 h, diluted with water and ethyl acetate and, extracted with ethyl acetate. The extracts were washed with brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue obtained was chromatographed on aluminum oxide in ethyl acetate:hexane (2:1) to give colorless crystals, 273.2 mg. This was recrystallized from acetone-isopropyl ether to give the titled compound as colorless crystals, m.p.175-176° C., 2654 mg. Yield 88%.

1. temperaturewith cooling in ice
2. extractionextracted with ethyl acetate
3. washThe extracts were washed with brine
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe residue obtained
7. customwas chromatographed on aluminum oxide in ethyl acetate:hexane (2:1)
8. customto give colorless crystals, 273.2 mg
9. customThis was recrystallized from acetone-isopropyl ether