تفاعل #6377

ord-6c29b27eab4d4e1eb2642d9e68152ba2

معادلة التفاعل

O
water
CC(=O)OCCc1ccc(OC(C)=O)cc1
4-acetoxyphenylmethylcarbinol acetate
CC(=O)OC(C)=O
acetic anhydride
O=P(O)(O)O
Phosphoric acid
O=P(O)(O)O
phosphoric acid
C=Cc1ccc(OC(C)=O)cc1
4-acetoxystyrene

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05247124uspto-grants-1993_09