反应详情

A Grignard reagent was prepared from 4-bromo-1-fluorobenzene (8.0 g), magnesium turnings (1.10 g), and iodine (one small crystal) in THF (40 ml). Oxetane (2.3 g) in THF (10 ml) was added at RT and the reaction mixture was heated at reflux overnight. The cooled solution was poured into aqueous saturated NH4Cl (100 ml), extracted with ER (2×150 ml) and the combined, dried (Na2SO4) extracts were evaporated. The residual oil was purified by flash chromatography over silica gel (Merck 9285, 5.0 cm wide column), eluting with ER-CX (1:5→1:3). The resultant oil was further purified by distillation to give the title compound (3.15 g) as a colourless oil, b.p. 150°/0.8 torr.

1. temperaturethe reaction mixture was heated
2. temperatureat reflux overnight
3. extractionextracted with ER (2×150 ml)
4. dry with materialdried (Na2SO4) extracts
5. customwere evaporated
6. customThe residual oil was purified by flash chromatography over silica gel (Merck 9285, 5.0 cm wide column)
7. washeluting with ER-CX (1:5→1:3)
8. distillationThe resultant oil was further purified by distillation