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Allyl bromide → 1,1-Bis(trifluoromethanesulfonyl)-3-butene

HRID 2211197
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인쇄 미리보기

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HRID 2211197 반응식
[CH2:1](Br)[CH:2]=[CH2:3].[Cl-].[Mg+2].[K+].[F:8][C:9]([F:22])([F:21])[S:10]([CH2:13][S:14]([C:17]([F:20])([F:19])[F:18])(=[O:16])=[O:15])(=[O:12])=[O:11].[Cl-].[Cl-]>C1COCC1>[F:19][C:17]([F:20])([F:18])[S:14]([CH:13]([S:10]([C:9]([F:8])([F:21])[F:22])(=[O:11])=[O:12])[CH2:3][CH:2]=[CH2:1])(=[O:15])=[O:16]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 7841Allyl bromideHCID 86749078Bis[(trifluoromethyl)sulfonyl] methane potassium magnesium chloride

생성물 1

HCID 193761101,1-Bis(trifluoromethanesulfonyl)-3-butene

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
70 °C

실험 절차

Next, 4,4-bis[(trifluoromethyl)sulfonyl]-1-butene was prepared by adding 3 ml of allyl bromide to 31.3 millimoles of the bis[(trifluoromethyl)sulfonyl] methane potassium magnesium chloride in 35 ml of THF. The mixture was stirred at 70° C. under reflux for 8 hours. After removal of solvent by distillation under reduced pressure, 50 ml of 3N hydrochloric acid was added to the residue and the aqueous solution was extracted with ethyl ether. The ethyl ether solution was dried with anhydrous MgSO4. The ethyl ether was removed from the solution and the product was distilled at 0.02 torr.

후처리

  1. temperatureunder reflux for 8 hours
  2. customAfter removal of solvent
  3. distillationby distillation under reduced pressure, 50 ml of 3N hydrochloric acid
  4. additionwas added to the residue
  5. extractionthe aqueous solution was extracted with ethyl ether
  6. dry with materialThe ethyl ether solution was dried with anhydrous MgSO4
  7. customThe ethyl ether was removed from the solution
  8. distillationthe product was distilled at 0.02 torr

출처 및 근거

ORD 기록
ord-f9d445e781a5474593383f9d5006ad80
출처 데이터셋
uspto-grants-1995_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05463005

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