반응 #74258

반응 방정식

2-vinyl-2-adamantanol

trimethyl orthoacetate

→

methyl 4-adamantylidenebutanoate

수율 82.0%

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

실험 절차

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%.

출처