Reaktion #8465

ord-9e3c8858286e46a0b9d74b5d94f6f030

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe resin was removed via filtration
  2. 2
    Sonstigethe filtrate evaporated
  3. 3
    SonstigeThe title compound was precipitated from ethyl acetate upon addition of hexanes
  4. 4
    Sonstigeused without further purification

Vorschrift

A solution of the product of Step B (6.77 g) and 2-amino-4-picoline (2.4 g) in ethanol (22 mL) was heated at 72° C. for 10 hours. The reaction mixture was cooled to ambient temperature and dissolved in methanol/dichloromethane and treated with Dowex® 550A basic resin until the pH of the mixture was 7. The resin was removed via filtration and the filtrate evaporated. The title compound was precipitated from ethyl acetate upon addition of hexanes and used without further purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07087757B2uspto-grants-2006_08