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Water → HCID 67328702, 화합물

HRID 1841832
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HRID 1841832 반응식
[F:1]/[C:2](/[Si](CC)(CC)CC)=[C:3](/[F:13])\[CH:4]1[CH2:9][CH2:8][CH:7]([CH2:10][CH2:11][CH3:12])[CH2:6][CH2:5]1.O.CCCC[N+](CCCC)(CCCC)CCCC.[F-]>C1COCC1.CC(OC)(C)C>[F:13]/[C:3](/[CH:4]1[CH2:9][CH2:8][CH:7]([CH2:10][CH2:11][CH3:12])[CH2:6][CH2:5]1)=[CH:2]/[F:1]
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HCID 962WaterHCID 2724141Tetrabutylammonium FluorideHCID 71074322[(Z)-1,2-difluoro-2-(4-propylcyclohexyl)vinyl]triethylsilane

생성물 1

HCID 67328702HCID 67328702, 화합물

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 15413tert-Butyl methyl ether용매

실험 절차

34.6 g (0.11 mol) of [(Z)-1,2-difluoro-2-(4-propylcyclohexyl)vinyl]triethylsilane are refluxed for 20 h in 900 ml of THF together with 45 ml of water and 160 ml of TBAF (0.16 mol, 1 M soln. in THF). The batch is diluted with MTBE and washed a number of times with water. The aqueous phases are extracted with MTBE, and the combined organic phases are washed with water and saturated sodium chloride solution. The solution is dried using sodium sulfate and concentrated under reduced pressure. The residue is purified by column chromatography (SiO2, pentane), giving 1-((E)-1,2-difluorovinyl)-4-propylcyclohexane as a colourless oil.

후처리

  1. washwashed a number of times with water
  2. extractionThe aqueous phases are extracted with MTBE
  3. washthe combined organic phases are washed with water and saturated sodium chloride solution
  4. customThe solution is dried
  5. concentrationconcentrated under reduced pressure
  6. customThe residue is purified by column chromatography (SiO2, pentane)

출처 및 근거

ORD 기록
ord-7de38795d58d4a14acea9041ea0f462f
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08945420B2

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