Reaktion #1568314

ord-79f81f02da5c4077bdf028d331b95206

Lösungsmittel

Reaktionsbedingungen

Temperatur
150°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was evaporated
  2. 2
    Sonstigethe residue was purified by column chromatography (0-40% EtOAc/hexanes+2% AcOH)

Vorschrift

A mixture of 1-cyano-4-hydroxy-7-phenylsulfanyl-isoquinoline-3-carboxylic acid butyl ester (50 mg, 0.13 mmol) and 3-amino-2,2-dimethyl-propionic acid methyl ester (52 mg, 0.40 mmol) in MeOH (2 mL) was heated at 150° C. in a microwave reactor for 3 h. The solvent was evaporated, and the residue was purified by column chromatography (0-40% EtOAc/hexanes+2% AcOH) to give 46 mg of the title compound. 1H NMR (CDCl3, 200 MHz): δ ppm=14.0 (s, 1H), 8.20-8.35 (m, 2H), 7.87 (d, 1H, J=1.2 Hz), 6.40-6.70 (m, 6H), 3.79 (s, 3H), 3.61 (d, 2H, J=7.0 Hz), 1.30 (s, 6H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09409892B2uspto-grants-2016_08