関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Phosphoric Acid | HCID 1004 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | 4-(2-Acetoxy-ethyl)phenyl Acetate | HCID 11195402 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 4-Ethenylphenyl acetate | HCID 75821 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05247124 |
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| 出典データセット | uspto-grants-1993_09 |
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| ORD ID | ord-6c29b27eab4d4e1eb2642d9e68152ba2 |
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| 出典メモ | uspto-grants-1993_09 |
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