Reaktion #1018477

ord-01d9ae7ed6cc4d74b2653719ce9b73f5

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was removed under reduced pressure
  2. 2
    Sonstigethe crude material was purified via preparative HPLC

Vorschrift

1-(Pyrimidin-2-yl)cyclopropanecarbaldehyde (0.11 g, 0.747 mmol), sulfur (40 mg, 1.24 mmol), and acetic acid (0.6 mL) were added to a solution of (R)-(1-(5,6-diaminopyridin-2-yl)piperidin-3-yl)(pyrrolidin-1-yl)methanone, prepared during the previous step, in ethanol. The reaction mixture was heated to 80° C. for 18 h. The solvent was removed under reduced pressure and the crude material was purified via preparative HPLC to afford the title compound (8 mg). MS (ES+APCI) (M+H) 418.2; LCMS retention time 3.273 min (Method S1).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09296745B2uspto-grants-2016_03