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

HRID 889142

반응식

HRID 889142 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-f012dcd74e9640939620c4371adbe3ec
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08252810B2

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