참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Catechol | HCID 289 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 2,2,2-Trichloroacetaldehyde hydrate | HCID 20528376 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 4-(2,2,2-Trichloro-1-hydroxyethyl)benzene-1,2-diol | HCID 14266062 | 52.5% |
반응 단계
To the solution of 440 g of 1,2-dihydroxybenzene dissolved in 1 L of methylene dichloride was added 1036 g of trichloroacetaldehyde monohydrate and then the reaction solution was cooled down to 0° C. 102 g of triethylamine was slowly added dropwise thereto. The reaction solution was warmed to room temperature, stirred for about 20 minutes, heated to 50° C. and then stirred for further 3 hours while maintaining the same temperature. After the reaction is completed, the reaction mixture was distilled under reduced pressure to remove methylene dichloride. The residue was dissolved in 4 L of ethylacetate, washed successively with 2400 ml of 0.5N-aqueous hydrochloric acid solution and 2 L of saturated saline, dried over anhydrous magnesium sulfate and then distilled under reduced pressure to remove the solvent and to obtain 540 g of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05541175 |
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| 출처 데이터셋 | uspto-grants-1996_07 |
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| ORD ID | ord-7f1f2144100f4a8e9624f9a6edc46410 |
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| 출처 메모 | uspto-grants-1996_07 |
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