関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | p-tert-Butylanisole | HCID 94750 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(5-Tert-butyl-2-hydroxyphenyl)ethan-1-one | HCID 263092 | — |
| 生成物 | HCID 13759988 | HCID 13759988 | — |
反応手順
To 7.40 g of aluminum chloride suspended in 100 ml of methylene chloride were added, under nitrogen, 8.20 g of 4-tert-butylanisole (prepared in Reference Example 1) dissolved in 50 ml of methylene chloride at 0° C. followed by dropwise addition of 3.92 ml of acetyl chloride dissolved in 50 ml of methylene chloride at the same temperature. The mixture was stirred at 20° C. for 30 minutes. The reaction mixture was concentrated at reduced pressure and poured into 200 ml of ice-water and extracted with diethyl ether. The extract was washed with water and saturated brine successively, dried over magnesium sulfate anhydride and concentrated at reduced pressure. The residue was chromatographed on silica gel column using a mixed solvent of methylene chloride and cyclohexane (1:2) as an eluting agent to give 5.30 g of the title compound and 3.79 g of 2-acetyl-4-tert-butylanisole. The physical properties of each compound are as follows.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04245099 |
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| 出典データセット | uspto-grants-1981_01 |
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| ORD ID | ord-0f0028d4dd42489e89ef36fcffb100e6 |
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| 出典メモ | uspto-grants-1981_01 |
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