Water → 2-Bromo-1-(3,4-dichlorophenyl)ethanone

HRID 248907

反応式

HRID 248907 の反応式
[Br:1]Br.[CH3:3][C:4]([C:6]1[CH:11]=[CH:10][C:9]([Cl:12])=[C:8]([Cl:13])[CH:7]=1)=[O:5].[Al+3].[Cl-].[Cl-].[Cl-].O>C(OCC)C>[Cl:13][C:8]1[CH:7]=[C:6]([CH:11]=[CH:10][C:9]=1[Cl:12])[C:4](=[O:5])[CH2:3][Br:1]

参加物

6

反応物 4

HCID 962WaterHCID 24408BromineHCID 75841Ethanone, 1-(3,4-dichlorophenyl)-HCID 6451240Aluminum(III) Chloride

生成物 1

HCID 2447512-Bromo-1-(3,4-dichlorophenyl)ethanone

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

Bromine in a quantity of 10.2 ml (0.2 mol) is added dropwise to a mixture of 37.8 g 3.4-dichloroacetophenone and approx. 1.0 g anhydrous AlCl3 in 600 ml dry diethylether while stirring and cooling in ice. After stirring for 0.5 hr at 0° C. and 1.5 hr at room temperature, 30 ml water are added slowly. The organic phase is separated, washed twice with water, dried and evaporated to dryness. A small amount of petroleum ether (40-60) is added to the residue and the mixture is stirred at approx. 0° C. The desired 3.4-dichlorophenacylbromide is obtained as a crystalline material in a yield of 39.8 g (74%); melting point 55°-58° C.; TLC (CH2Cl2)=0.5.

後処理

  1. temperaturecooling in ice
  2. stirringAfter stirring for 0.5 hr at 0° C. and 1.5 hr at room temperature
  3. customThe organic phase is separated
  4. washwashed twice with water
  5. customdried
  6. customevaporated to dryness
  7. additionA small amount of petroleum ether (40-60) is added to the residue
  8. stirringthe mixture is stirred at approx. 0° C

出典と根拠

ORDレコード
ord-8cc3378f8f4c456abf138b1e58aecd9c
出典データセット
uspto-grants-1993_05
特許番号
US05212197

関連ノート

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