Water → 1-(Chloromethyl)-4-(fluoromethyl)benzene

HRID 889142ノート

反応式

HRID 889142 の反応式
[Cl:1][CH2:2][C:3]1[CH:10]=[CH:9][C:6]([CH2:7]O)=[CH:5][CH:4]=1.O.C(=O)([O-])O.[Na+].CN(S(F)(F)[F:21])C>ClCCl>[Cl:1][CH2:2][C:3]1[CH:10]=[CH:9][C:6]([CH2:7][F:21])=[CH:5][CH:4]=1

参加物

6

反応物 4

HCID 962WaterHCID 123203Sulfur, trifluoro(N-methylmethanaminato)-HCID 516892Sodium BicarbonateHCID 5107660[4-(Chloromethyl)phenyl]methanol

生成物 1

HCID 189264181-(Chloromethyl)-4-(fluoromethyl)benzene

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

After dissolving 4-(chloromethyl)benzyl alcohol (5.00 g) in dichloromethane (90 ml), dimethylaminosulfur trifluoride (8.28 ml) was added at room temperature and the mixture was stirred for one day. Water was added to the reaction mixture, and then a saturated aqueous solution of sodium hydrogencarbonate was added and extraction was performed with ethyl acetate. The organic layer was washed with brine and dried over anhydrous magnesium sulfate. After filtration, the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography to obtain the title compound (2.94 g).

後処理

  1. additionwas added at room temperature
  2. extractionextraction
  3. washThe organic layer was washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationAfter filtration
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-f012dcd74e9640939620c4371adbe3ec
出典データセット
uspto-grants-2012_08
特許番号
US08252810B2

反応ノート

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