N,N,N',N'-Tetramethylethylenediamine → HCID 178467770、化合物

HRID 2265786ノート

反応式

HRID 2265786 の反応式
[F:1][C:2]([F:17])([S:13]([O-:16])(=[O:15])=[O:14])[C:3]([F:12])([F:11])[C:4]([F:10])([F:9])[C:5]([F:8])([F:7])[F:6].O[C:19]1[CH:24]=[CH:23][C:22]([S+:25]([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)=[CH:21][CH:20]=1.[C:38](=[O:41])([O-])[O-].[K+].[K+].CN(C)[CH2:46][CH2:47]N(C)C.[CH:52]([O:54][CH2:55][CH2:56][CH2:57][CH2:58][CH2:59]CCCCl)=[CH2:53]>CS(C)=O>[F:17][C:2]([F:1])([S:13]([O-:16])(=[O:15])=[O:14])[C:3]([F:11])([F:12])[C:4]([F:10])([F:9])[C:5]([F:8])([F:7])[F:6].[CH:52]([O:54][CH:55]([CH2:56][CH2:57][CH2:58][CH3:59])[CH2:46][CH2:47][CH2:38][O:41][SH+:25]([C:22]1[CH:21]=[CH:20][CH:19]=[CH:24][CH:23]=1)([C:26]1[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=1)[C:32]1[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=1)=[CH2:53]

参加物

6

反応物 4

HCID 8037N,N,N',N'-TetramethylethylenediamineHCID 11430Potassium CarbonateHCID 22481373HCID 22481373、化合物HCID 566088708-Chlorooctyl vinyl ether

生成物 1

HCID 178467770HCID 178467770、化合物

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
80 °C

実験手順

4-Hydroxyphenyldiphenylsulfonium perfluorobutanesulfonate (2.67 g), potassium carbonate (0.78 g), and N,N,N′,N′-tetramethylethylenediamine (0.05 g) were dissolved in dimethyl sulfoxide (13.3 g). Subsequently, 8-chlorooctyl vinyl ether (1.05 g) was added to the resultant solution, followed by heating to 80° C. and stirring for 15 hours. The resultant reaction mixture was cooled to 30° C. or lower. After removal of solid matter through filtration, water (13.3 g) was added to the filtrate, and the aqueous layer was washed thrice with hexane (7.96 g). Dichloromethane (10.6 g) and water (g) were added to the washed aqueous layer, followed by stirring for extraction of a target substance into the dichloromethane layer. The organic layer was repeatedly washed with distilled water until the pH of the separated aqueous layer became 7. The solvent was removed by means of a rotary evaporator, to thereby yield 2.53 g of a brown oily substance. Through 1H-NMR analysis and ion chromatography, this substance was identified to be 4-vinyloxyoctoxyphenyldiphenylsulfonium perfluorobutanesulfonate.

後処理

  1. customThe resultant reaction mixture
  2. temperaturewas cooled to 30° C.
  3. customAfter removal of solid matter
  4. filtrationthrough filtration, water (13.3 g)
  5. additionwas added to the filtrate
  6. washthe aqueous layer was washed thrice with hexane (7.96 g)
  7. additionDichloromethane (10.6 g) and water (g) were added to the washed aqueous layer
  8. stirringby stirring for extraction of a target substance into the dichloromethane layer
  9. washThe organic layer was repeatedly washed with distilled water until the pH of the separated aqueous layer
  10. customThe solvent was removed by means of a rotary evaporator

出典と根拠

ORDレコード
ord-4a6e3143517e49bbae05ababcc3b2cc6
出典データセット
uspto-grants-2010_12
特許番号
US07858287B2

反応ノート

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