関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 4-Chlorobenzoyl chloride | HCID 8501 | — |
| 反応物 | 4-Ethylphenol | HCID 31242 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | 1,1,2,2-Tetrachloroethane | HCID 6591 | — |
| 生成物 | (4-Chlorophenyl)(5-ethyl-2-hydroxyphenyl)methanone | HCID 12562655 | — |
反応手順
Aluminium chloride (267 g) was added in portions over 30 minutes to a stirred solution of 4-ethylphenol (122.1 g.) and 4-chlorobenzoyl chloride (140 ml.) in dry 1,1,2,2-tetrachloroethane (800 ml.). The mixture was heated at 105° C. for 22 hours with stirring, and on cooling a mixture of ice (600 g) and concentrated hydrochloric acid was added slowly. A vigorous reaction occurred and some material was lost. The remaining material was separated, the aqueous fraction extracted twice with chloroform (200 ml.), and the combined organic layers evaporated to a dark oil which was distilled in vacuo giving two main fractions: B (17.4 g) 150°-160° C. at 0.3 mmHg; C (110.8 g) 160°-168° C. at 0.3 mmHg. The title compound was crystallised by cooling to -20° C. and recrystallised from n-hexane at 0° C. to give a yellow crystalline solid m.p. 35°-8° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04141995 |
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| 出典データセット | uspto-grants-1979_02 |
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| ORD ID | ord-24f31516e4db42cf9af6f18d87063f3e |
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| 出典メモ | uspto-grants-1979_02 |
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