반응 #51258

ord-8fce33b15a5c4c0e9f5294a5695d02da

반응 방정식

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
수율 90.5%
NSOOc1ccc(-n2nc(C(N)=O)c3ccc4ccc(N)cc4c32)cc1
8-amino-1-{4-[(aminothio)peroxy]phenyl}-1H-benzo[g]indazole-3-carboxamide
수율 90.5%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도at reflux for 16 h
  2. 2
    여과The mixture was then filtered
  3. 3
    농축concentrated
  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
    여과was collected by filtration
  7. 7
    기타dried

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06849653B2uspto-grants-2005_02