Perfluorobutanesulfonic acid → Diphenyliodanium nonafluorobutane-1-sulfonate

HRID 970264

반응식

HRID 970264 반응식
[Br-].[C:2]1([I+:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[F:15][C:16]([F:31])([F:30])[C:17]([F:29])([F:28])[C:18]([F:27])([F:26])[C:19]([F:25])([F:24])[S:20]([OH:23])(=[O:22])=[O:21]>[Ag]=O.CO>[F:31][C:16]([F:15])([F:30])[C:17]([F:28])([F:29])[C:18]([F:26])([F:27])[C:19]([F:24])([F:25])[S:20]([O-:23])(=[O:22])=[O:21].[C:9]1([I+:8][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1

참가 물질

5

반응물 2

HCID 67815Perfluorobutanesulfonic acidHCID 73871Iodonium, diphenyl-, bromide (1:1)

생성물 1

HCID 16216934Diphenyliodanium nonafluorobutane-1-sulfonate수율 79.3%

시약·촉매·용매 2

HCID 92152Silver(II) oxide촉매HCID 887Methanol용매

실험 절차

To 100 ml of methanol, 3.61 g (0.01 mole) of diphenyliodonium bromide and 1.62 g (0.007 mole) of silver oxide were suspended, then the mixture was reacted at room temperature for 2 hours. To the reaction solution, 4.2 g (0.014 mole) of nonafluorobutanesulfonic acid was added drop-wise at room temperature, followed by reacting at the same temperature for 2 hours while stirring. The thus obtained reaction mixture was filtered and concentrated under reduced pressure, followed by purifying 6.4 g of the residue by column chromatography [Wako gel, C-200; eluent of methylene chloride/methanol=9/1 (v/v)], to obtain 4.6 g of diphenyliodonium nonafluorobutanesulfonate as a colorless crystal. The thus obtained crystal was named acid generator B1. The measurement results of melting point and NMR of acid generator B1 are shown bellow.

후처리

  1. customthe mixture was reacted at room temperature for 2 hours
  2. customThe thus obtained reaction mixture
  3. filtrationwas filtered
  4. concentrationconcentrated under reduced pressure
  5. customby purifying 6.4 g of the residue by column chromatography [Wako gel, C-200; eluent of methylene chloride/methanol=9/1 (v/v)]

출처 및 근거

ORD 기록
ord-6c2008237a64455bb97166bc766e048d
출처 데이터셋
uspto-grants-2007_12
특허 번호
US07312014B2

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