Reaktion #83812

ord-8543d2bf211b46a087be799b6515f8ea

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeA procedure similar to that described in Preparation 43
  2. 2
    Sonstigewere reacted
  3. 3
    Sonstigeas described in Preparation 43
  4. 4
    Sonstigethe resulting crude product was purifying by column chromatography through silica gel
  5. 5
    workup.ADDITIONby volume mixture of ethyl acetate and methanol as the eluent
  6. 6
    Sonstigewas then crystallized by trituration with ethyl acetate

Vorschrift

A procedure similar to that described in Preparation 43 was repeated, except that 7.50 g of 3-amino-6-benzyloxy-2-methylaminopyridine (prepared as described in Preparation 93) and 7.46 g of glycolic acid were reacted. After working up the product as described in Preparation 43 , the resulting crude product was purifying by column chromatography through silica gel, using a 10:1 by volume mixture of ethyl acetate and methanol as the eluent, and was then crystallized by trituration with ethyl acetate, to give 4.10 g of the title compound, melting at 133°-135° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05624935uspto-grants-1997_04