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Tetrahydrofuran → 1-Bromo-2-ethylsulfanyl-4-trifluoromethylsulfanylbenzene

HRID 1750049
ノート
印刷プレビュー

反応式

HRID 1750049 の反応式
[CH2:1]([S-:3])[CH3:2].[Na+].[Br:5][C:6]1[CH:11]=[CH:10][C:9]([S:12][C:13]([F:16])([F:15])[F:14])=[CH:8][C:7]=1F.C1COCC1.C(=O)(O)[O-].[Na+]>CN(C=O)C>[Br:5][C:6]1[CH:11]=[CH:10][C:9]([S:12][C:13]([F:16])([F:15])[F:14])=[CH:8][C:7]=1[S:3][CH2:1][CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8028TetrahydrofuranHCID 516892Sodium BicarbonateHCID 4459711Sodium ethanethiolateHCID 1180356764-Bromo-3-fluorophenyl trifluoromethyl sulphide

生成物 1

HCID 1180355631-Bromo-2-ethylsulfanyl-4-trifluoromethylsulfanylbenzene収率 58.3%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

0.21 g of sodium ethanethiolate (80%) was added to a mixture of 0.55 g of l-bromo-2-fluoro-4-trifluoromethylsulfanylbenzene and 4 ml of THF under ice cooling, and the mixture was stirred at room temperature for 30 minutes. 2 mL of DMF was added to the reaction mixture, and the mixture was stirred at 80° C. for 2 hours. A saturated aqueous sodium bicarbonate solution was added to the cooled reaction mixture, and the mixture was extracted with ethyl acetate and then dried with anhydrous sodium sulfate. The mixture was concentrated under reduced pressure, and the resulting residue was applied to a silica gel column chromatography to obtain 0.37 g of 1-bromo-2-ethylsulfanyl-4-trifluoromethylsulfanylbenzene.

後処理

  1. stirringthe mixture was stirred at 80° C. for 2 hours
  2. extractionthe mixture was extracted with ethyl acetate
  3. dry with materialdried with anhydrous sodium sulfate
  4. concentrationThe mixture was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-09172ec6784f44fda24172d803031bb5
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09156838B2

反応ノート

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