Hydrogen Bromide → 19-Bromo-1,1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8-heptadecafluorononadecane
反応式
[F:1][C:2]([F:37])([C:33]([F:36])([F:35])[F:34])[C:3]([F:32])([F:31])[C:4]([F:30])([F:29])[C:5]([F:28])([F:27])[C:6]([F:26])([F:25])[C:7]([F:24])([F:23])[C:8]([F:22])([F:21])[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19]O.[BrH:38].S(=O)(=O)(O)O>O>[Br:38][CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][C:8]([F:21])([F:22])[C:7]([F:23])([F:24])[C:6]([F:25])([F:26])[C:5]([F:27])([F:28])[C:4]([F:29])([F:30])[C:3]([F:31])([F:32])[C:2]([F:1])([F:37])[C:33]([F:34])([F:35])[F:36]参加物
5
反応条件
- 温度
- 100 °C
実験手順
To a mixture of 29.0 g of crude 11-(heptadecafluorooctyl)-1-undecanol and 250 mL of 48% 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 of silica with hexanes. Concentration of the eluent afforded 20.2 g of crude 1-bromo-11-(heptadecafluorooctyl)undecane as a nearly white solid, which was used without further purification.
後処理
- extractionThe mixture was extracted with hexanes
- washthe combined organic phases were washed with saturated aqueous sodium bicarbonate
- dry with materialdried over anhydrous magnesium sulfate
- concentrationThe solution was concentrated to a dark liquid, which
- washwas eluted through 3 inches of silica with hexanes
出典と根拠
- ORDレコード
- ord-9aa331cdd6d144129208ee13d902ab0b
- 出典データセット
- uspto-grants-2004_11
- 特許番号
- US06824882B2
反応ノート
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