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Acetone → 2-Oxo-3,3-dimethylbutyl-thiacyclopentanium trifluoromethanesulfonate

HRID 394430
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HRID 394430 반응식
[F:1][C:2]([F:8])([F:7])[S:3]([O-:6])(=[O:5])=[O:4].[K+].CC(C)=O.C(OCC)C.[Br-].[O:20]=[C:21]([C:28]([CH3:31])([CH3:30])[CH3:29])[CH2:22][S+:23]1[CH2:27][CH2:26][CH2:25][CH2:24]1>C(#N)C>[F:1][C:2]([F:8])([F:7])[S:3]([O-:6])(=[O:5])=[O:4].[O:20]=[C:21]([C:28]([CH3:31])([CH3:30])[CH3:29])[CH2:22][S+:23]1[CH2:27][CH2:26][CH2:25][CH2:24]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 180AcetoneHCID 3283Diethyl EtherHCID 225645781-(3,3-Dimethyl-2-oxobutyl)thiolan-1-ium bromideHCID 23664779Potassium Trifluoromethanesulfonate

생성물 1

HCID 181759402-Oxo-3,3-dimethylbutyl-thiacyclopentanium trifluoromethanesulfonate수율 87.8%

시약·촉매·용매 1

HCID 6342
Acetonitrile
용매
2회

실험 절차

In a 300 ml three-necked flask, 2 g of 2-oxo-3,3-dimethylbutyl-thiacyclopentanium bromide obtained in Example 1 was dissolved in 20 ml of acetonitrile. To the solution, a solution prepared by dissolving 1.69 g of a potassium trifluoromethanesulfonate salt in 50 ml of acetonitrile was added dropwise. After stirring for three hours, the deposited potassium bromide was removed by filtration and acetonitrile was distilled off under reduced pressure by an evaporator. The residue was dissolved in chloroform and the insoluble matter was removed by filtration. Chloroform in the filtrate was distilled off under reduced pressure to obtain a transparent viscous liquid. To the transparent viscous liquid, 5 ml of acetone was added and the solution was added dropwise to 300 ml of diethyl ether. The deposited white crystal was collected by filtration and then recrystallized from ethyl acetate. The resulting white powder was dried under reduced pressure at 30° C. for six hours to obtain 2.21 g of 2-oxo-3,3-dimethylbutyl-thiacyclopentanium trifluoromethanesulfonate (yield: 87.7%).

후처리

  1. customTo the solution, a solution prepared
  2. additionwas added dropwise
  3. customthe deposited potassium bromide was removed by filtration and acetonitrile
  4. distillationwas distilled off under reduced pressure by an evaporator
  5. dissolutionThe residue was dissolved in chloroform
  6. customthe insoluble matter was removed by filtration
  7. distillationChloroform in the filtrate was distilled off under reduced pressure
  8. customto obtain a transparent viscous liquid
  9. filtrationThe deposited white crystal was collected by filtration
  10. customrecrystallized from ethyl acetate
  11. customThe resulting white powder was dried under reduced pressure at 30° C. for six hours

출처 및 근거

ORD 기록
ord-95bef059a97f4998bf22597655fbac5c
출처 데이터셋
uspto-grants-2003_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06602647B2

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