Hydrogen Peroxide → 1-Cyclohexylsulfonyl-3,3-dimethyl-2-butanone

HRID 129371

반응식

HRID 129371 반응식
[CH2:1]1[CH2:6][CH2:5][CH:4]([SH:7])[CH2:3][CH2:2]1.[OH-:8].[K+].Br[CH2:11][C:12](=[O:17])[C:13]([CH3:16])([CH3:15])[CH3:14].[OH:18]O>C(O)C.[O-][W]([O-])(=O)=O.[Na+].[Na+]>[CH:4]1([S:7]([CH2:11][C:12](=[O:17])[C:13]([CH3:16])([CH3:15])[CH3:14])(=[O:18])=[O:8])[CH2:5][CH2:6][CH2:1][CH2:2][CH2:3]1

참가 물질

7

반응물 4

HCID 784Hydrogen PeroxideHCID 14797Potassium HydroxideHCID 15290CyclohexanethiolHCID 21642Bromopinacolone

생성물 1

HCID 229086321-Cyclohexylsulfonyl-3,3-dimethyl-2-butanone수율 28.7%

시약·촉매·용매 2

HCID 26052Sodium tungstate촉매HCID 702Ethanol용매

실험 절차

To cyclohexylthiol (23 g, 0.198 mole), a solution of potassium hydroxide (13.7 g, 0.207 mole) in ethanol (80 ml) was added dropwise at 15° C., followed by stirring at the same temperature for 24 hours. After 1-bromo-3,3-dimethyl-2-butanone (35.4 g, 0.198 mole) was added dropwise to the reaction mixture at 10°-15° C. and continued to stir at 20° C. for 5 hours, sodium tungstate (2.5 g) was added. Then, 30% hydrogen peroxide (220 g, 1.96 mole) was added dropwise at 45°-50° C. and reacted with stirring at 60°-80° C. for 30 hours. After cooling, the reaction mixture was extracted with methylene chloride (300 ml×1), the organic layer was separated, dried over anhydrous MgSO4 and evaporated to obtain 14 g of residual crude 1-cyclohexylsulfonyl-3,3-dimethyl-2-butanone as a pale yellow oil.

후처리

  1. stirringto stir at 20° C. for 5 hours
  2. customreacted
  3. stirringwith stirring at 60°-80° C. for 30 hours
  4. temperatureAfter cooling
  5. extractionthe reaction mixture was extracted with methylene chloride (300 ml×1)
  6. customthe organic layer was separated
  7. dry with materialdried over anhydrous MgSO4
  8. customevaporated

출처 및 근거

ORD 기록
ord-5f9e35a15e6347eb878ff043c31f1985
출처 데이터셋
uspto-grants-1995_11
특허 번호
US05468589

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