Hydrogen Peroxide → 1-(Isopropylsulfonyl)propan-2-one

HRID 129375

反応式

HRID 129375 の反応式
[CH3:1][CH:2]([SH:4])[CH3:3].[OH-:5].[K+].Cl[CH2:8][C:9](=[O:11])[CH3:10].[OH:12]O>C(O)C.[O-][W]([O-])(=O)=O.[Na+].[Na+]>[CH3:1][CH:2]([S:4]([CH2:8][C:9]([CH3:10])=[O:11])(=[O:12])=[O:5])[CH3:3]

参加物

7

反応物 4

HCID 784Hydrogen PeroxideHCID 63642-PropanethiolHCID 6571ChloroacetoneHCID 14797Potassium Hydroxide

生成物 1

HCID 229086371-(Isopropylsulfonyl)propan-2-one収率 71.9%

試薬・触媒・溶媒 2

HCID 26052Sodium tungstate触媒HCID 702Ethanol溶媒

実験手順

To 2-propanethiol (12.2 g, 0.16 mole), a solution of potassium hydroxide (11.5 g, 0.174 mole) in ethanol (100 ml) was added dropwise at 15° C. or lower, and continued to stir at the same temperature for 24 hours. Then chloroacetone (23.1 g, 0.25 mole) was added dropwise at 10°-15° C., and reacted with stirring at 20° C. for 4 hours. To this mixture, sodium tungstate (0.8 g) was added, 30% hydrogen peroxide (36 g, 0.32 mole) was added dropwise at 45°-55° C., and reacted with stirring at room temperature for 14 hours. The reaction mixture was extracted with methylene chloride (200 ml). The organic layer was washed with H2O, dried over anhydrous MgSO4 and evaporated to give 18.9 g of residual crude 1-(1-methylethylsulfonyl)acetone as a brownish yellow oil.

後処理

  1. customreacted
  2. stirringwith stirring at 20° C. for 4 hours
  3. customreacted
  4. stirringwith stirring at room temperature for 14 hours
  5. extractionThe reaction mixture was extracted with methylene chloride (200 ml)
  6. washThe organic layer was washed with H2O
  7. dry with materialdried over anhydrous MgSO4
  8. customevaporated

出典と根拠

ORDレコード
ord-cd3cc7551858402b927a8ff0ae3afcfc
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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