반응 #74259

반응 방정식

2-vinyl-2-propanol

trimethyl orthoacetate

→

methyl 5-methyl-4-hexenate

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 60 to 65° 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 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%.

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