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

HRID 2211197
ノート
印刷プレビュー

反応式

HRID 2211197 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
70 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f9d445e781a5474593383f9d5006ad80
出典データセット
uspto-grants-1995_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05463005

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート