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Phosphorus tribromide → 1-(Bromomethyl)-2-(trifluoromethyl)benzene

HRID 326701
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HRID 326701 반응식
P(Br)(Br)[Br:2].[F:5][C:6]([F:16])([F:15])[C:7]1[CH:14]=[CH:13][CH:12]=[CH:11][C:8]=1[CH2:9]O>C1(C)C=CC=CC=1>[F:5][C:6]([F:16])([F:15])[C:7]1[CH:14]=[CH:13][CH:12]=[CH:11][C:8]=1[CH2:9][Br:2]
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참가 물질

4

반응물 2

HCID 24614Phosphorus tribromideHCID 676662-(Trifluoromethyl)benzylic alcohol

생성물 1

HCID 1230571-(Bromomethyl)-2-(trifluoromethyl)benzene

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

A solution of 30 ml of phosphorus tribromide in 60 ml of absolute toluene was added dropwise at 20°-30° C. to a solution of 14 g of o-trifluoromethylbenzyl alcohol in 80 ml of absolute toluene. Subsequently, the reaction mixture was stirred at room temperature for 2 hours, the toluene was distilled under reduced pressure, the residue was dissolved in methylene chloride, treated with water and the mixture was adjusted to pH 8.0 with potassium hydrogen carbonate. The aqueous phase was extracted three times with CH2Cl2 and the organic phases were washed twice with water and once with saturated NaCl solution, dried over Na2SO4 and evaporated under reduced pressure. o-Trifluoromethylbenzyl bromide was obtained as the residue.

후처리

  1. distillationthe toluene was distilled under reduced pressure
  2. dissolutionthe residue was dissolved in methylene chloride
  3. additiontreated with water
  4. extractionThe aqueous phase was extracted three times with CH2Cl2
  5. washthe organic phases were washed twice with water and once with saturated NaCl solution
  6. dry with materialdried over Na2SO4
  7. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-0569fc5a788c47769d676e97dce0c4c1
출처 데이터셋
uspto-grants-1993_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05270313

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