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Aluminum(III) Chloride → 7-Bromo-3,4-dihydro-1-benzoxepin-5(2H)-one

HRID 2096603
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HRID 2096603 반응식
[Br:1][C:2]1[CH:14]=[CH:13][C:5]([O:6][CH2:7][CH2:8][CH2:9][C:10](Cl)=[O:11])=[CH:4][CH:3]=1.[Al+3].[Cl-].[Cl-].[Cl-]>C(Cl)Cl>[Br:1][C:2]1[CH:14]=[CH:13][C:5]2[O:6][CH2:7][CH2:8][CH2:9][C:10](=[O:11])[C:4]=2[CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6451240Aluminum(III) ChlorideHCID 58424408HCID 58424408, 화합물

생성물 1

HCID 106815487-Bromo-3,4-dihydro-1-benzoxepin-5(2H)-one수율 103.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
0 °C

실험 절차

A solution of 4-(4-bromophenoxy)butanoyl chloride (27.6 g, 100 mmol) in DCM (200 mL) was added dropwise to a solution of AlCl3 (50 g, 0.38 mol) in DCM (100 mL) at 0° C. within 40 minutes, the mixture was stirred at 0° C. for 1.5 hours, and then stirred at room temperature overnight. the mixture was added to a stirred mixture of concentrated hydrochloric (500 mL) and ice, and then stirred for 1.5 hours. The mixture was extracted with DCM, washed with NaHCO3, dried over Na2SO4 and concentrated to give crude 7-bromo-3,4-dihydrobenz o[b]oxepin-5(2H)-one (25 g, 96%).

후처리

  1. stirringstirred at room temperature overnight
  2. additionthe mixture was added to a stirred mixture of concentrated hydrochloric (500 mL) and ice
  3. stirringstirred for 1.5 hours
  4. extractionThe mixture was extracted with DCM
  5. washwashed with NaHCO3
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-2ec1cd41412a4edc899f09a2146678b4
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08450308B2

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