[CH:1]([O:12][CH:13]([CH2:15][CH3:16])[CH3:14])(OC(CC)C)OC(CC)C.[C:17]1(=O)[CH2:22][CH2:21]C[CH2:19][CH2:18]1.CC(O)CC>[Fe](Cl)(Cl)Cl>[CH3:14][CH:13]([O:12][C:1]1[CH2:21][CH2:22][CH2:17][CH2:18][CH:19]=1)[CH2:15][CH3:16]A mixture containing 116.2 g (0.5 mol) of tri(2-butyl) orthoformate, 49.10 g (0.5 mol) of cyclohexanone and 3.7 g (0.05 mol) of 2-butanol was stirred at room temperature (25° C.) and 0.2 g (1 mmol) of reagent grade iron (III) chloride was added. The temperature of the reaction mixture rose to about 35° C. due to the exotherm and was heated and maintained at about at 50° C. until gas-chromatographic analysis indicated that the reaction was complete. After removing the by-products 2-butyl formate and 2-butanol by distillation under reduced pressure, the resulting residue was subsequently distilled to provide 1-(2-butoxy)-1-cyclohexene (bp 86° C. @2 mm Hg) as a colorless liquid; the yield was 89.4% with a purity exceeding 99%.
불러오는 중…
