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(3-Bromopropyl)benzene → 4-(3-bromopropyl)benzoyl Chloride

HRID 346248
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HRID 346248 반응식
[Br:1][CH2:2][CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.C(Cl)(=O)[C:12]([Cl:14])=[O:13].[Cl-].[Al+3].[Cl-].[Cl-]>ClC=C(Cl)Cl>[Br:1][CH2:2][CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][C:8]([C:12]([Cl:14])=[O:13])=[CH:7][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 12503(3-Bromopropyl)benzeneHCID 65578Oxalyl chlorideHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 113690154-(3-bromopropyl)benzoyl Chloride수율 97.3%

시약·촉매·용매 1

HCID 6575Trichloroethylene용매

실험 절차

To a cold (ice bath) stirred solution of 50.0 g (0.25 mole) of 1-bromo-3-phenylpropane (Aldrich) and 31.9 g (0.25 mole) of oxalyl chloride in 300 mL of trichloroethylene was added, portionwise, 33.3 g (0.25 mole) of aluminum chloride. The reaction mixture was stirred for 0.5 hr and then poured into ice water. The layers were separated and the aqueous layer was extracted with three 100 mL portions of methylene chloride. The combined organic layers were washed twice with 200 mL portions of water and dried (magnesium sulfate). The solvents were evaporated under reduced pressure to leave 63.6 g (97%) of 4-(3-bromopropyl)benzoyl chloride as an oil. To a solution of the acid chloride in 120 mL of dry benzene was added 60 mL of absolute ethanol and the mixture was heated at reflux for 3 hr. The solvents were evaporated under reduced pressure to give 63.4 g (93.5%) of an oil. The oil was purified by chromatography (3.5×90 cm glass column, 200 g of silica gel, benzene-hexane, 1:1). Fractions containing the desired component were combined and the solvents evaporated under reduced pressure to give 60.6 g (89%) of the title compound as a pale yellow oil.

후처리

  1. additionwas added
  2. customThe layers were separated
  3. extractionthe aqueous layer was extracted with three 100 mL portions of methylene chloride
  4. washThe combined organic layers were washed twice with 200 mL portions of water
  5. dry with materialdried (magnesium sulfate)
  6. customThe solvents were evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-7656ab29036248cd9fcb524e8e91563d
출처 데이터셋
uspto-grants-1991_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05061720

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