참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetyl chloride | HCID 6367 | — |
| 반응물 | p-tert-Butylanisole | HCID 94750 | — |
| 반응물 | Aluminum(III) Chloride | HCID 6451240 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 1-(5-Tert-butyl-2-hydroxyphenyl)ethan-1-one | HCID 263092 | — |
| 생성물 | HCID 13759988 | HCID 13759988 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04245099 |
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| 출처 데이터셋 | uspto-grants-1981_01 |
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| ORD ID | ord-0f0028d4dd42489e89ef36fcffb100e6 |
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| 출처 메모 | uspto-grants-1981_01 |
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