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

HRID 23572

反应方程式

HRID 23572 反应方程式
[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

参与物

5

反应物 3

HCID 784Hydrogen PeroxideHCID 656671焦亚硫酸钠HCID 225750461,2-Diphenyl-4-(4-methylphenyl)-3,5-pyrazolidinedione

产物 1

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

试剂、催化剂与溶剂 1

HCID 176醋酸溶剂

实验过程

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%).

后处理

  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%)

来源与证据

ORD记录
ord-baeea72672b647a4baeb6e9fbd6b854b
来源数据集
uspto-grants-2005_02
专利号
US06852749B1

关联笔记

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