반응 #6407

반응 방정식

triiodophenol

2,2,3,4,4-pentafluoro-3,4-dibromo-butyryl chloride

→

material

수율 99.0%

(2,4,6-triiodophenyl)-2,2,3,4,4-pentafluoro-3,4-dibromo-butyrate

수율 99.0%

용매

pyridine

반응 조건

후처리

1. 1
   기타did not rise above 65° C
2. 2
   workup.STIRRINGThe mixture was stirred at 50° C. for an additional 30 minutes
3. 3
   기타overnight
4. 4
   기타at room temperature
5. 5
   세척The mixture was washed in a separatory funnel three times with 500 ml of DI water
6. 6
   여과filtered through a column of silica
7. 7
   기타the solvent evaporated
8. 8
   기타The material was then chromatographed on a column of silica using FREON 113 (trichlorotrifluroethane) as eluent

실험 절차

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