Hydrogen Peroxide → 1,2-Diphenyl-4-hydroxy-4-(4-methylphenyl)-3,5-pyrazolidinedione

HRID 23572

反応式

HRID 23572 の反応式
[C:1]1([N:7]2[C:11](=[O:12])[CH:10]([C:13]3[CH:18]=[CH:17][C:16]([CH3:19])=[CH:15][CH:14]=3)[C:9](=[O:20])[N:8]2[C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.OO.S(S([O-])=O)([O-])(=O)=[O:30].[Na+].[Na+]>C(O)(=O)C>[C:1]1([N:7]2[C:11](=[O:12])[C:10]([OH:30])([C:13]3[CH:18]=[CH:17][C:16]([CH3:19])=[CH:15][CH:14]=3)[C:9](=[O:20])[N:8]2[C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

5

反応物 3

HCID 784Hydrogen PeroxideHCID 656671Sodium PyrosulfiteHCID 225750461,2-Diphenyl-4-(4-methylphenyl)-3,5-pyrazolidinedione

生成物 1

HCID 97988671,2-Diphenyl-4-hydroxy-4-(4-methylphenyl)-3,5-pyrazolidinedione

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture of 1,2-diphenyl-4-(4-methylphenyl)-3,5-pyrazolidinedione (1.10 g; 3.2 =mol), 35% H2O2 (0.47 ml; 5.5 mmol), and acetic acid (40 ml) was stirred 16 days at room temperature. Sodium metabisulfite (1.0 g) was added and excess acetic acid evaporated off. The residue was dissolved in hot ethyl acetate (25 ml) and benzene (25 ml) and filtered. After cooling to room temperature, the mixture was filtered and the residue recrystallized from 50% aqueous ethanol (20 ml) to give 0.58 g (53%).

後処理

  1. customexcess acetic acid evaporated off
  2. dissolutionThe residue was dissolved in hot ethyl acetate (25 ml)
  3. filtrationbenzene (25 ml) and filtered
  4. temperatureAfter cooling to room temperature
  5. filtrationthe mixture was filtered
  6. customthe residue recrystallized from 50% aqueous ethanol (20 ml)
  7. customto give 0.58 g (53%)

出典と根拠

ORDレコード
ord-baeea72672b647a4baeb6e9fbd6b854b
出典データセット
uspto-grants-2005_02
特許番号
US06852749B1

関連ノート

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