反应详情

温度

115 °C

A distillation column-provided four-necked flask having a volume of 100 mL, which was equipped with a dropping funnel, a thermometer, a stirring device and a reflux ratio regulator, was charged with 25.0 g (140.2 mmoles) of 2-vinyl-2-adamantanol, 30.3 g (280.5 mmoles) of trimethyl orthoacetate and 0.2 g (2.8 mmoles) of propionic acid, and the internal temperature was raised to 115° C. Heating was continued for 16 hours while removing a fraction of not higher than 65° C. from a column top of the distillation column. At that time, 0.2 g (2.8 mmoles) of propionic acid was added 16 times every one hour. The reaction mixture was concentrated at 110° C. under atmospheric pressure to obtain 26.9 g (115.0 mmoles) of methyl 4-adamantylidenebutanoate. The yield was 82.0%.

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. concentrationThe reaction mixture was concentrated at 110° C. under atmospheric pressure