反应详情

To a tetrahydrofuran (74 mL) solution of the compound 9 (7.3 g) was added a 1 M tetrabutylammonium fluoride/tetrahydrofuran solution (27 mL), and the mixture was stirred for 3 hours. The reaction liquid was diluted with ethyl acetate (380 mL), washed with water (740 mL) and a saturated saline (380 mL). Further the aqueous layer was extracted with ethyl acetate (100 mL). The organic layers were combined, dried with anhydrous sodium sulfate, and concentrated. The resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=2:1). The resulting compound was purified again by silica gel column chromatography (dichloromethane:ethyl acetate=4:1→ethyl acetate) to obtain a titled compound (3.24 g) having the following physical property values.

1. customThe reaction liquid
2. washwashed with water (740 mL)
3. extractionFurther the aqueous layer was extracted with ethyl acetate (100 mL)
4. dry with materialdried with anhydrous sodium sulfate
5. concentrationconcentrated
6. customThe resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=2:1)
7. customThe resulting compound was purified again by silica gel column chromatography (dichloromethane:ethyl acetate=4:1→ethyl acetate)