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1,3-Dibromobenzene → 2-Bromo-1-(2,4-dibromophenyl)-1-propanone

HRID 1450252
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HRID 1450252 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[Br:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([Br:12])[CH:7]=1.[Br:13][CH:14]([CH3:18])[C:15](Br)=[O:16]>C(=S)=S>[Br:13][CH:14]([CH3:18])[C:15]([C:9]1[CH:10]=[CH:11][C:6]([Br:5])=[CH:7][C:8]=1[Br:12])=[O:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 79271,3-DibromobenzeneHCID 79047Propanoyl bromide, 2-bromo-HCID 6451240Aluminum(III) Chloride

생성물 1

HCID 189677542-Bromo-1-(2,4-dibromophenyl)-1-propanone수율 76%

시약·촉매·용매 1

HCID 6348Carbon Disulfide용매

실험 절차

15 g of aluminium chloride are added with caution, at 0° C., to 25 g of 1,3-dibromobenzene in 250 ml of carbon disulphide, and 22.86 g of 2-bromopropionyl bromide are then run in slowly. The mixture is maintained at reflux for 8 hours, then the carbon disulphide is evaporated off under vacuum and the reaction medium is poured onto crushed ice. The product is extracted twice with heptane, dried, evaporated to dryness and then purified on a column of silica, using a mixture of cyclohexane and ethyl acetate (10:1 v/v) as eluent, to give the expected product.

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후처리

  1. temperatureThe mixture is maintained
  2. temperatureat reflux for 8 hours
  3. customthe carbon disulphide is evaporated off under vacuum
  4. additionthe reaction medium is poured
  5. customonto crushed ice
  6. extractionThe product is extracted twice with heptane
  7. customdried
  8. customevaporated to dryness
  9. custompurified on a column of silica
  10. additiona mixture of cyclohexane and ethyl acetate (10:1 v/v) as eluent

출처 및 근거

ORD 기록
ord-3e2bbc48b6d24aafa22a7efc9850e394
출처 데이터셋
uspto-grants-1997_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05602132

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