반응 #51850

ord-baeea72672b647a4baeb6e9fbd6b854b

반응 방정식

Cc1ccc(C2C(=O)N(c3ccccc3)N(c3ccccc3)C2=O)cc1
1,2-diphenyl-4-(4-methylphenyl)-3,5-pyrazolidinedione
OO
H2O2
O=S([O-])S(=O)(=O)[O-].[Na+].[Na+]
Sodium metabisulfite
Cc1ccc(C2(O)C(=O)N(c3ccccc3)N(c3ccccc3)C2=O)cc1
1,2-Diphenyl-4-hydroxy-4-(4-methylphenyl)-3,5-pyrazolidinedione

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타excess acetic acid evaporated off
  2. 2
    workup.DISSOLUTIONThe residue was dissolved in hot ethyl acetate (25 ml)
  3. 3
    여과benzene (25 ml) and filtered
  4. 4
    온도After cooling to room temperature
  5. 5
    여과the mixture was filtered
  6. 6
    기타the residue recrystallized from 50% aqueous ethanol (20 ml)
  7. 7
    기타to give 0.58 g (53%)

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%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06852749B1uspto-grants-2005_02