반응 #6377

반응 방정식

water

4-acetoxyphenylmethylcarbinol acetate

acetic anhydride

Phosphoric acid

phosphoric acid

→

4-acetoxystyrene

용매

acetic acid

반응 조건

후처리

1. 1
   온도A flask heated by hot oil
2. 2
   workup.ADDITIONwas added
3. 3
   온도The hot oil temperature was maintained at about 220° C. to about 230° C.
4. 4
   온도the reaction mass temperature in the hot flask was maintained at about 180° C. to about 200° C
5. 5
   온도The vacuum pump maintained a vacuum in the flask at about 80 mm Hg

실험 절차

A flask heated by hot oil was fitted with a chilled water overhead condenser, a thermowell with a thermocouple, an overhead stirrer and a vacuum pump. Crude APMC-Ether (20 grams) containing 78.2 weight percent APMC-Ether, 7.2 weight percent APMC and 3.9 weight percent 4-acetoxyphenylmethylcarbinol acetate (sometimes referred to herein as "APMC-Acetate") was mixed in another flask with six (6.0) grams of acetic anhydride. Phosphoric acid (0.022 grams) having a concentration of 85 weight percent that corresponds to 0.32 moles of pure phosphoric acid per 100 moles of APMC-Ether was added to said mixture. The resultant mixture was fed to the hot flask at a rate of 1.2 grams per minute. The hot oil temperature was maintained at about 220° C. to about 230° C. and the reaction mass temperature in the hot flask was maintained at about 180° C. to about 200° C. The vacuum pump maintained a vacuum in the flask at about 80 mm Hg. 4-acetoxystyrene and acetic acid were produced in the hot flask.

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