반응 #74257

반응 방정식

1-vinyl-1-cyclohexanol

trimethyl orthoacetate

→

methyl 4-cyclohexylidenebutanoate

수율 86.0%

반응 조건

후처리

1. 1
   workup.DISTILLATIONA distillation
2. 2
   기타column-provided four-necked flask
3. 3
   기타was equipped with a dropping funnel
4. 4
   온도Heating
5. 5
   기타while removing a fraction of not higher than 65° C.
6. 6
   workup.DISTILLATIONfrom a column top of the distillation column
7. 7
   workup.DISTILLATIONthe reaction solution was distilled in vacuo
8. 8
   기타Fractions of from 120 to 130° C./1.2 kPa were collected

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%.

출처