Reaktion #532872

ord-5b1ce173aa6d44cd896f8bd6c1f31b9f

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGthe reaction mixture was stirred 25 h at rt
  2. 2
    SonstigeThe reaction mixture was purified by prep

Vorschrift

A solution of [4-(8-bromo-2-oxo-2,3-dihydro-imidazo[4,5-c]quinolin-1-yl)-3-methyl-pyrazol-1-yl]-acetic acid (Stage 101.1.2, 178 mg, 0.443 mmol), DIPE (0.232 ml, 1.33 mmol), TPTU (223 mg, 0.752 mmol) in DMA (5 ml) was stirred at rt for 5 min, then was added N-methylpiperazine (0.1 ml, 0.90 mmol). The reaction mixture was stirred 19 h at rt and then was added N-methylpiperazine (0.1 ml, 0.90 mmol) and the reaction mixture was stirred 25 h at rt. The reaction mixture was purified by prep. HPLC to give the title compound as an off-white solid. (HPLC: tR 1.98 min (Method A); M+H=484, 486 MS-ES)

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08476294B2uspto-grants-2013_07