Trimethyl orthoacetate → 4-Cyclohexylidene butanoic acid, methyl ester
반응식
[CH:1]([C:3]1(O)[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1)=[CH2:2].[C:10](OC)([O:14]C)([O:12][CH3:13])[CH3:11]>C(O)(=O)CC>[C:3]1(=[CH:1][CH2:2][CH2:11][C:10]([O:12][CH3:13])=[O:14])[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1참가 물질
4
반응 조건
- 온도
- 115 °C
실험 절차
A distillation column-provided four-necked flask having a volume of one liter, which was equipped with a dropping funnel, a thermometer, a stirring device and a reflux ratio regulator, was charged with 250 g (1.922 moles) of 1-vinyl-1-cyclohexanol, 415.6 g (3.843 moles) of trimethyl orthoacetate and 1.4 g (0.019 moles) of propionic acid, and the internal temperature was raised to 115° C. Heating was continued for 12 hours while removing a fraction of not higher than 65° C. from a column top of the distillation column. After confirming the disappearance of 1-vinyl-1-cyclohexanol by a gas chromatographic analysis of the reaction solution, the reaction solution was distilled in vacuo. Fractions of from 120 to 130° C./1.2 kPa were collected to obtain 301.2 g (1.653 moles) of methyl 4-cyclohexylidenebutanoate. The yield was 86.0%.