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3-Chloro-2-methyl-1-propene → 2-Methyl-3-(2,5-dimethylphenylthio)propane

HRID 368941
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HRID 368941 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][C:3]=1[SH:9].[CH2:10](Cl)[C:11](=[CH2:13])[CH3:12].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH3:10][CH:11]([CH2:13][S:9][C:3]1[CH:4]=[C:5]([CH3:8])[CH:6]=[CH:7][C:2]=1[CH3:1])[CH3:12]
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참가 물질

5

반응물 3

HCID 112413-Chloro-2-methyl-1-propeneHCID 11430Potassium CarbonateHCID 776152,5-Xylenethiol

생성물 1

HCID 234506662-Methyl-3-(2,5-dimethylphenylthio)propane수율 89%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A 100-ml eggplant type flask was charged with 6.9 g (50 mmol) of 2,5-dimethylthiophenol, 5.5 g (60 mmol, 1.2 equivalents) of methallyl chloride which was a halogenated olefin, 6.9 g (50 mmol, 1 equivalent) of potassium carbonate and 30 ml of acetone, and the mixture was refluxed under heat for 1 hour. The reaction mixture was allowed to cool, insolubles were removed by filtration, and the acetone was distilled off. The resultant residue was re-dispersed in n-hexane and washed with a saturated sodium chloride aqueous solution. An organic layer was dried over anhydrous sodium sulfate, and then the solvent was distilled off to give 8.6 g (yield 89%) of 2-methyl-3-(2,5-dimethylphenylthio)-propane.

후처리

  1. temperaturethe mixture was refluxed
  2. temperatureunder heat for 1 hour
  3. temperatureto cool
  4. custominsolubles were removed by filtration
  5. distillationthe acetone was distilled off
  6. additionThe resultant residue was re-dispersed in n-hexane
  7. washwashed with a saturated sodium chloride aqueous solution
  8. dry with materialAn organic layer was dried over anhydrous sodium sulfate
  9. distillationthe solvent was distilled off

출처 및 근거

ORD 기록
ord-322e7a040c5a4baeba3754e9f6f551dd
출처 데이터셋
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06136755

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