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

HRID 2351559노트

반응식

HRID 2351559 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

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온도
-30 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-54f787ba4f5a4186a7ea3e390e9be1cc
출처 데이터셋
uspto-grants-1989_10
특허 번호
US04873329

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