Реакция #2337

ord-49e1ae57538b4195be3dcdaff27940ff

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураwas heated
  2. 2
    Температураto reflux
  3. 3
    ТемператураHeating
  4. 4
    ДругоеThe reaction mixture was evaporated until a slight turbidity
  5. 5
    ДругоеOn further cooling, a precipitate formed which
  6. 6
    Другоеwas collected
  7. 7
    Промывкаwashed with ethyl acetate
  8. 8
    Другоеdried

Методика

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%.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05728701uspto-grants-1998_03