참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Boron trifluoride | HCID 6356 | — |
| 반응물 | 2,6-Dimethylphenol | HCID 11335 | — |
| 반응물 | Dimethyl 4,4'-biphenyldicarboxylate | HCID 13099 | — |
| 반응물 | Hydrofluoric Acid | HCID 14917 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 4,4'-Bis(3,5-dimethyl-4-hydroxybenzoyl)biphenyl | HCID 23454579 | — |
반응 단계
4,4'-Dicarbomethoxybiphenyl (67 g, 0.25 mole) and 2,6-dimethylphenol (61 g, 0.50 mole) were charged to a one-liter Hastalloy C® shaker tube. The tube was cooled and charged with hydrogen fluoride (200 g) and boron trifluoride (75 g). The tube was heated to 50° C. and shaken at 50° C. for 4 hr. It was then cooled and vented, and the contents, an orange solid in an orange solution, were allowed to evaporate in the hood. The orange solid that resulted was stirred in 2 l. of water, warmed, and isolated by filtration of the warm mixture. The precipitate was stirred in 2 l. of water, warmed, and neutralized with sodium bicarbonate. The solid was isolated by filtration of the warm solution, washed with water, and air dried to afford crude 4,4'-bis(3,5-dimethyl-4-hydroxybenzoyl)biphenyl in a yield of 107.6 g (96%), as a salmon-colored powder.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04276226 |
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| 출처 데이터셋 | uspto-grants-1981_06 |
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| ORD ID | ord-d8d0c2d8025441c489643199082246b4 |
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| 출처 메모 | uspto-grants-1981_06 |
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