Hydrogen Bromide → 19-Bromo-1,1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8-heptadecafluorononadecane

HRID 1760496노트

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HRID 1760496 반응식
[C:1]([C:5]([C:8]([C:11]([C:14]([C:17]([C:20]([C:23]([CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36]O)([F:25])[F:24])([F:22])[F:21])([F:19])[F:18])([F:16])[F:15])([F:13])[F:12])([F:10])[F:9])([F:7])[F:6])([F:4])([F:3])[F:2].[BrH:38].S(=O)(=O)(O)O>O>[C:1]([C:5]([C:8]([C:11]([C:14]([C:17]([C:20]([C:23]([CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][Br:38])([F:25])[F:24])([F:22])[F:21])([F:19])[F:18])([F:16])[F:15])([F:13])[F:12])([F:10])[F:9])([F:7])[F:6])([F:4])([F:3])[F:2]

참가 물질

5

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온도
100 °C

실험 절차

To a mixture of 29.0 g (0.049) of CF3(CF2)7(CH2)10CH2OH and 250 mL of 48 percent by weight aqueous hydrobromic acid was slowly added 25 mL of concentrated sulfuric acid. The reaction mixture was heated at 100° C. for 18 hr and poured into 1 liter of water. The mixture was extracted with hexanes, and the combined organic phases were washed with saturated aqueous sodium bicarbonate and dried over anhydrous magnesium sulfate. The solution was concentrated to a dark liquid, which was eluted through 3 inches (8 cm) of silica with hexanes. Concentration of the eluent yielded 20.2 g of CF3(CF2)7(CH2)10CH2Br as a nearly white solid, which was used without further purification.

후처리

  1. extractionThe mixture was extracted with hexanes
  2. washthe combined organic phases were washed with saturated aqueous sodium bicarbonate
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationThe solution was concentrated to a dark liquid, which
  5. washwas eluted through 3 inches (8 cm) of silica with hexanes

출처 및 근거

ORD 기록
ord-4fee1fa98df34143861aaa7a0089a4ed
출처 데이터셋
uspto-grants-2005_01
특허 번호
US06841079B2

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