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

HRID 399622
ノート
印刷プレビュー

反応式

HRID 399622 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6348Carbon Disulfide溶媒

実験手順

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 is 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.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  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. customis purified on a column of silica
  10. additiona mixture of cyclohexane and ethyl acetate (10:1 v/v) as eluent

出典と根拠

ORDレコード
ord-acee76ca33654733933892fa063250da
出典データセット
uspto-grants-1998_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05821255

反応ノート

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