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

HRID 23572

반응식

HRID 23572 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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%).

후처리

  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%)

출처 및 근거

ORD 기록
ord-baeea72672b647a4baeb6e9fbd6b854b
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06852749B1

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