Реакция #2338

ord-35a8c2a4b4bc4caeaaf6b411adca67fe

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеevaporated to dryness
  2. 2
    ДругоеThe residue was triturated with water (2 ml)
  3. 3
    Фильтрацияfiltered
  4. 4
    ДругоеThe solid thus obtained
  5. 5
    Другоеwas recrystallised from water

Методика

A solution of methyl 4-[2-(piperazin-2-one-1-yl)acetyl]-phenoxyacetate (0.347 g), 4-chloropyridine hydrochloride (0.19 g) and triethylamine (0.178 g) in water (8 ml) and dioxan (1 ml) was heated on a steam bath for 2 hours and then evaporated to dryness. The residue was triturated with water (2 ml) and filtered. The solid thus obtained was recrystallised from water to give the title compound (0.187 g), m.p. 275°-277° C.; NMR(d6DMSO δ 8.33(2H,d), 8.0(2H,d), 7.21(2H,d), 7.1(2H,d), 4.97(2H,s), 4.81(2H,s), 3.94(2H,m), 3.59(2H,m); m/e 370(H+H)+ ; calculated for C19H20N3O5Cl. 0.75 H2O: C, 54.4; H, 5.0; N, 10.0. Found: C, 54.5; H, 5.3; N, 9.5%.

Источник

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