Reaktion #51258

ord-8fce33b15a5c4c0e9f5294a5695d02da

Reaktionsgleichung

NSOOc1ccc(-n2nc(C(N)=O)c3c2-c2cc(N)ccc2CC3)cc1
product
NSOOc1ccc(-n2nc(C(N)=O)c3c2-c2cc(N)ccc2CC3)cc1
8-amino-1-{4-[(aminothio)peroxy]phenyl}-4,5-dihydro-1H-benzo[g]indazole-3-carboxamide
CN1CCCC1=O
NMP
NSOOc1ccc(-n2nc(C(N)=O)c3ccc4ccc(N)cc4c32)cc1
title compound
Ausbeute 90.5%
NSOOc1ccc(-n2nc(C(N)=O)c3ccc4ccc(N)cc4c32)cc1
8-amino-1-{4-[(aminothio)peroxy]phenyl}-1H-benzo[g]indazole-3-carboxamide
Ausbeute 90.5%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturat reflux for 16 h
  2. 2
    FiltrationThe mixture was then filtered
  3. 3
    Einengenconcentrated
  4. 4
    workup.ADDITIONThe residue was diluted with methanol (10 mL)
  5. 5
    workup.ADDITIONadded to water, after 1 h the resulting precipitate
  6. 6
    Filtrationwas collected by filtration
  7. 7
    Sonstigedried

Vorschrift

The product of Example 4b (1 g) and 5% Pd/C (300 mg) suspended in cumene (50 mL) and NMP (5 mL) was heated at reflux for 16 h. The mixture was then filtered and concentrated. The residue was diluted with methanol (10 mL) and added to water, after 1 h the resulting precipitate was collected by filtration and dried to yield the title compound (0.9 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06849653B2uspto-grants-2005_02