Reacción #1792009

ord-5feccf620b88479ba556e3f48bce9ab7

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturacooled
  2. 2
    ConcentraciónThe mixture was concentrated to dryness
  3. 3
    Otrothe residue was triturated with cold 1N HCl
  4. 4
    Otrocrystallized from benzene

Procedimiento

Isobutyryl chloride (455 mg., 4.26 mmoles) was added to a stirred, cooled (ice-water) mixture of 6,7-dihydro-10-hydroxy-4-oxo-4H-pyrimido[2,1-a]isoquinoline-3-carboxylic acid (1.03 g., 3.87 mmoles) and triethylamine (785 mg., 7.75 mmoles) in methylene chloride (20 ml.). The mixture was concentrated to dryness and the residue was triturated with cold 1N HCl, and then crystallized from benzene to give the title compound 0.81 g. (64% yield). The product was recrystallized successively from ethyl acetate and methanol to give the analytical sample, m.p. 183°-185°.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04127720uspto-grants-1978_11