Reacción #2337

ord-49e1ae57538b4195be3dcdaff27940ff

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturawas heated
  2. 2
    Temperaturato reflux
  3. 3
    TemperaturaHeating
  4. 4
    OtroThe reaction mixture was evaporated until a slight turbidity
  5. 5
    OtroOn further cooling, a precipitate formed which
  6. 6
    Otrowas collected
  7. 7
    Lavadowashed with ethyl acetate
  8. 8
    Otrodried

Procedimiento

A mixture of the product from Example 26 (1.5 g) and methanol (80 ml) was heated to reflux with stirring, and solid pyridine hydrochloride (0.5 g) was added. Heating was stopped and ethyl acetate (10 ml) was added. The reaction mixture was evaporated until a slight turbidity was observed. On further cooling, a precipitate formed which was collected, washed with ethyl acetate and dried to give the title compound (1.33 g) as a beige solid: m.p.>240° C. (dec); NMR (d6 -DMSO) δ 1.90 (2H, m), 2.36 (2H, t), 3.17 (4H, m), 3.83 (4H, m), 3.91 (2H, t), 6.89 (4H, q), 7.26 (2H, d), 8.25 (2H, d), 12.1 (1H, br), 13.75 (1H, br); m/Z 342 (M+H)+ ; calculated for C19H23N3O3. 1.0 HCl: C, 60.4%; H, 6.4%; N, 11.1%; found: C, 60.0%; H, 6.4%, N, 10.8%.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05728701uspto-grants-1998_03