Reaktion #933882

ord-52c9154fdfca406b8dc6ee68491ad955

Reaktionsbedingungen

Temperatur
45°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was removed by evaporation

Vorschrift

Following the procedure of Step 2 Example 331 a 0.168 g (1.17 mmol) of 1,5-dioxa-8-azaspiro[5.4]decane, from Step 2 Example 14, was reacted with 0.300 g (0.78 mmol) of 1-(2,4-difluorophenyl)-7-chloro-6-fluoro-1,8-naphthyridine-3-carboxylic acid ethyl ester by heating at 40° C. instead of 45° C. for 10 instead of 24 hours. The solvent was removed by evaporation to afford the title product which was purified by column chromatography over silica gel (0% increasing to 4% methanol/methylene chloride) to afford 0.252 g of the title compound. The ester was not further purified, but was taken directly to the next step.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05137892uspto-grants-1992_08