反应详情

温度

115 °C

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 50.0 g (580.5 mmoles) of 2-vinyl-2-propanol, 139.5 g (1,161.0 mmoles) of trimethyl orthoacetate and 1.3 g (17.4 mmoles) 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 2-vinyl-2-propanol by a gas chromatographic analysis of the reaction solution, the reaction solution was distilled in vacuo. Fractions of from 60 to 65° C./1.2 kPa were collected to obtain 62.2 g (437.1 mmoles) of methyl 5-methyl-4-hexenate. The yield was 75.3%.

1. distillationA distillation
2. customcolumn-provided four-necked flask
3. customwas equipped with a dropping funnel
4. temperatureHeating
5. customwhile removing a fraction of not higher than 65° C.
6. distillationfrom a column top of the distillation column
7. distillationthe reaction solution was distilled in vacuo
8. customFractions of from 60 to 65° C./1.2 kPa were collected