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

HRID 129371

反応式

HRID 129371 の反応式
[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

参加物

7

反応物 4

HCID 784Hydrogen PeroxideHCID 14797Potassium HydroxideHCID 15290CyclohexanethiolHCID 21642Bromopinacolone

生成物 1

HCID 229086321-Cyclohexylsulfonyl-3,3-dimethyl-2-butanone収率 28.7%

試薬・触媒・溶媒 2

HCID 26052Sodium tungstate触媒HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5f9e35a15e6347eb878ff043c31f1985
出典データセット
uspto-grants-1995_11
特許番号
US05468589

関連ノート

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