반응식
I[Br:2].BrBr.[F:5][C:6](I)([F:29])[C:7]([F:28])([F:27])[C:8]([F:26])([F:25])[C:9]([F:24])([F:23])[C:10]([F:22])([F:21])[C:11]([F:20])([F:19])[C:12]([F:18])([F:17])[C:13]([F:16])([F:15])[F:14]>>[F:5][C:6]([Br:2])([F:29])[C:7]([F:28])([F:27])[C:8]([F:26])([F:25])[C:9]([F:24])([F:23])[C:10]([F:22])([F:21])[C:11]([F:20])([F:19])[C:12]([F:18])([F:17])[C:13]([F:16])([F:15])[F:14]참가 물질
실험 절차
With reference to FIG. 1, and H-shaped tube equipped with a Dimroth condenser and a Dimroth condenser having an IBr withdrawing cock was attached to a 500-ml four-necked flask. Into the flask were placed 200 ml (747 mM) of perfluorooctyl iodide (PFOI) and 5.0 ml (97.1 mM) of bomine, and the mixture was heated at 150° to 155° C. and irradiated with a 500-W visible light lamp. After the reaction mixture started to reflux, 49.5 ml (972 mM) of bromine was added dropwise to the mixture at a rate of 0.2 ml/min over a period of about 4 hours. The resulting IBr was drawn off at a suitable time through the IBr withdrawing Dimroth condenser. The reaction was continued for 5 hours, and the reaction mixture was thereafter cooled and washed with a 5% aqueous solution (200 ml) of sodium hydroxide to obtain 344.9 g (92.5% in yield) of perfluorooctyl bromide.
후처리
- customWith reference to FIG. 1, and H-shaped tube equipped with a Dimroth condenser
- customwas attached to a 500-ml four-necked flask
- temperaturethe mixture was heated at 150° to 155° C.
- customirradiated with a 500-W visible light lamp
- temperatureto reflux
- temperaturethe reaction mixture was thereafter cooled
- washwashed with a 5% aqueous solution (200 ml) of sodium hydroxide
출처 및 근거
- ORD 기록
- ord-417cc42ce2af4639a3f1a6947628937f
- 출처 데이터셋
- uspto-grants-1997_11
- 특허 번호
- US05688379
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