참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 2,4,6-Triiodophenol | HCID 11862 | — |
| 반응물 | 3,4-Dibromo-2,2,3,4,4-pentafluorobutanoyl chloride | HCID 14533537 | — |
| 용매 | Pyridine | HCID 1049 | — |
| 생성물 | (2,4,6-Triiodophenyl)-2,2,3,4,4-pentafluoro-3,4-dibromo-butyrate | HCID 14533541 | 99% |
반응 단계
100 grams of triiodophenol were dissolved in 100 ml of pyridine with warming to 50° C. 75 grams of 2,2,3,4,4-pentafluoro-3,4-dibromo-butyryl chloride were added dropwise through a dropping funnel with stirring at such a rate that the temperature did not rise above 65° C. The mixture was stirred at 50° C. for an additional 30 minutes, then overnight at room temperature. The mixture was washed in a separatory funnel three times with 500 ml of DI water, then filtered through a column of silica and the solvent evaporated. The material was then chromatographed on a column of silica using FREON 113 (trichlorotrifluroethane) as eluent. Chromatography on silica gave 75.5 grams of material 99% pure. The material solidified at room temperature and has a melting point of 50° C. I.R.(ν, in cm-1)=3050, 3090 (Ar--H); 1800 (C=O); 1570, 1415 (Ar C=C). m/e 62 (47%, C5H2); 69 (18%, CF3); 129 (22%, CF2Br); 131 (70%, CF2Br and C3F5); 189 (60%, C5H2I); 344 (56%, C6H2I2O); 471 (100%, C6H2I3O).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05248432 |
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| 출처 데이터셋 | uspto-grants-1993_09 |
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| ORD ID | ord-6ff4bdd1e3964baaae33d90c3af4eb2c |
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| 출처 메모 | uspto-grants-1993_09 |
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