反应详情

To a stirring solution of 8-[(4-fluorophenyl)methyl]-1,4-dioxaspiro[4.5]decane (18 g, 72 mmol) in 100 mL of THF was added 1 M hydrogen chloride in water (70 mL) followed by conc hydrogen chloride (50 mL). The reaction was heated to reflux for 5 h and then cooled to room temperature. The reaction was conc in vacuo to 120 mL and then extracted with ethyl acetate (3×100 mL). The organic layers were combined, washed with sat sodium bicarbonate, brine, dried over sodium sulfate, and conc in vacuo to a colorless oil. The oil was purified by flash chromatography (SiO2, 10:1 hexanes:ethyl acetate) to yield 9.6 g of a colorless oil. MS (ESI) 207 (M+H).

1. temperatureThe reaction was heated
2. temperatureto reflux for 5 h
3. extractionextracted with ethyl acetate (3×100 mL)
4. washwashed with sat sodium bicarbonate, brine
5. dry with materialdried over sodium sulfate
6. customThe oil was purified by flash chromatography (SiO2, 10:1 hexanes:ethyl acetate)