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Water → 4-(2-Bromoethyl)benzaldehyde

HRID 323807
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HRID 323807 반응식
C[O:2][CH:3](Cl)Cl.[CH2:6]([Br:14])[CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.O>C(Cl)Cl.[Ti](Cl)(Cl)(Cl)Cl>[Br:14][CH2:6][CH2:7][C:8]1[CH:13]=[CH:12][C:11]([CH:3]=[O:2])=[CH:10][CH:9]=1
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참가 물질

6

반응물 3

HCID 962WaterHCID 7666Phenethyl bromideHCID 21004Methane, dichloromethoxy-

생성물 1

HCID 110851354-(2-Bromoethyl)benzaldehyde

시약·촉매·용매 2

HCID 24193Titanium Tetrachloride촉매HCID 6344Dichloromethane용매2회

실험 절차

To a solution of dichloromethyl methyl ether (62 ml) in methylene chloride (40 ml) was added titanium tetrachloride (75 ml) over 10 minutes under a nitrogen atmosphere at 4-5° C. Then, a solution of phenethyl bromide (85 ml) in methylene chloride (50 ml) was added thereto over 50 minutes at 5-7° C. and the mixture was stirred for 5 hours while gradually raising the temperature of the mixture to room temperature. Water (200 ml) was added to the reaction mixture over 1 hour and the mixture was extracted with chloroform (200 ml). The chloroform layer was washed with water, a saturated aqueous sodium bicarbonate solution and saturated brine, dried over anhydrous sodium sulfate and the solvent was distilled away under reduced pressure to give a brown oily substance (167 g). The obtained brown oily substance was purified by silica gel column chromatography (eluent; hexane: ethyl acetate=20:1) to give 4-(2-bromoethyl)benzaldehyde (32.3 g) as a yellow solid, melting point 50-52° C.

후처리

  1. extractionthe mixture was extracted with chloroform (200 ml)
  2. washThe chloroform layer was washed with water
  3. dry with materiala saturated aqueous sodium bicarbonate solution and saturated brine, dried over anhydrous sodium sulfate
  4. distillationthe solvent was distilled away under reduced pressure
  5. customto give a brown oily substance (167 g)
  6. customThe obtained brown oily substance was purified by silica gel column chromatography (eluent; hexane: ethyl acetate=20:1)

출처 및 근거

ORD 기록
ord-a6e20d09f11d400dbf970895d2eefd4c
출처 데이터셋
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06214873B1

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