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

HRID 1086842ノート

反応式

HRID 1086842 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 The residue
  6. customwas purified by chromatography on a silica gel column

出典と根拠

ORDレコード
ord-b66594a2a8b5460c85a003e5be7a552e
出典データセット
uspto-grants-1991_07
特許番号
US05032592

反応ノート

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