反应详情

The 3-trifluoromethylbenzylphosphonochloridic acid ethyl ester of Example 4 (0.2 g, 0.7 mmol) was dissolved in 20 mL of CH2Cl2 and added slowly at 0° C. to a mixture of 1.0 mmol of allyl alcohol and 1.0 of mmol triethylamine in 20 mL of CH2Cl2. The reaction mixture was stirred for 5 hours and then diluted with H2O. The aqueous phase was further extracted 3 times with CH2Cl2. The organic extracts were combined and, after drying with anhydrous Na2SO4, were evaporated to give the crude product as an oil. Purification by column chromatography on silica gel using ethyl acetate/hexane (2.5:1) yielded 0.14 g (63%) of analytically pure product as a colorless oil. D.C.I.M.S.[MH+ 309].

1. extractionThe aqueous phase was further extracted 3 times with CH2Cl2
2. dry with materialafter drying with anhydrous Na2SO4
3. customwere evaporated
4. customto give the crude product as an oil
5. customPurification by column chromatography on silica gel
6. customyielded 0.14 g (63%) of analytically pure product as a colorless oil