Reaktion #68453

ord-fc76c502eb6d407db4f6272427ad0b0f

Lösungsmittel

Reaktionsbedingungen

Temperatur
50°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenConcentrated
  2. 2
    EinengenConcentrated
  3. 3
    Temperaturwith cooling
  4. 4
    Sonstigewas isolated by filtration
  5. 5
    SonstigeUsed without further purification

Vorschrift

A mixture of 1-(6-chloropyridazin-3-yl)hydrazine (0.372 g, 2.57 mmol), 1-hydroxy-7-aza-benzotriazole (0.350 g, 2.57 mmol), EDC (0.641 g, 3.34 mmol), 2-(7-methoxyquinolin-4-yloxy)acetic acid (0.600 g, 2.57 mmol) and diisopropylethylamine (1.34 ml, 7.72 mmol) in DMF (20 mL) was allowed to stir at 50° C. for 2 h. Concentrated. Reconstitued in MeCN (30 mL). Concentrated with cooling. Product crashed out of solution and was isolated by filtration. Used without further purification. (ESI, pos. ion) m/z: 234.1 (M+H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08524900B2uspto-grants-2013_09