Bromoform → 1,1-Dibromo-2-(3,4-dichlorophenyl)cyclopropane

HRID 2351559ノート

反応式

HRID 2351559 の反応式
CC(C)([O-])C.[K+].[Cl:7][C:8]1[CH:9]=[C:10]([CH:15]=[CH2:16])[CH:11]=[CH:12][C:13]=1[Cl:14].[CH:17]([Br:20])(Br)[Br:18]>O>[Br:18][C:17]1([Br:20])[CH2:16][CH:15]1[C:10]1[CH:11]=[CH:12][C:13]([Cl:14])=[C:8]([Cl:7])[CH:9]=1

参加物

5

反応物 3

HCID 5558BromoformHCID 748693,4-DichlorostyreneHCID 23665647Potassium tert-butoxide

生成物 1

HCID 198185011,1-Dibromo-2-(3,4-dichlorophenyl)cyclopropane

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
-30 °C

実験手順

Potassium t-butoxide (5.1 g.) was added to a stirred mixture of 3,4-dichlorophenylethylene (6.1 g.), bromoform (8.9 g.) and petroleum ether (b.p. 60°-80° C.; 100 ml.) which was cooled to -30° C., and the mixture was stirred at that temperature for 30 minutes, then at laboratory temperature for 17 hours and then poured into water. The mixture was extracted with ethyl acetate and the extract was washed with saturated aqueous sodium chloride solution, dried over magnesium sulphate and evaporated to dryness under reduced pressure. The residue was purified by chromatography on a silica gel column using petroleum ether (b.p. 40°-60° C.) as eluant, and there was thus obtained as an oil 1,1-dibromo-2-(3,4-dichlorophenyl)cyclopropane.

後処理

  1. waitat laboratory temperature for 17 hours
  2. extractionThe mixture was extracted with ethyl acetate
  3. washthe extract was washed with saturated aqueous sodium chloride solution
  4. dry with materialdried over magnesium sulphate
  5. customevaporated to dryness under reduced pressure
  6. customThe residue was purified by chromatography on a silica gel column

出典と根拠

ORDレコード
ord-54f787ba4f5a4186a7ea3e390e9be1cc
出典データセット
uspto-grants-1989_10
特許番号
US04873329

反応ノート

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