Реакция #3393

ord-c3b0e2987bf6463288457f21739f34ea

Реагенты

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураheated
  2. 2
    Температураat reflux until no starting material
  3. 3
    Фильтрацияfiltered
  4. 4
    Концентрированиеconcentrated
  5. 5
    ДругоеThe residue was triturated with hot hexane (5×1 L)
  6. 6
    Концентрированиеconcentrated
  7. 7
    Другоеto afford 48 g (54%)

Методика

2-Chloro-5-nitropyridine (100 g, 0.656 mol, Aldrich), KF (84.1 g, 1.448 mol), Ph4PBr (95.3 g, 0.227 mol) and acetonitrile (1.5 L) were combined and heated at reflux until no starting material remained. The volume was reduced to 750 mL, and the mixture was diluted with 2 L of ether, filtered and concentrated. The residue was triturated with hot hexane (5×1 L). The hexane extracts were combined and concentrated to afford 48 g (54%). 1H NMR (CDCl3, 300 MHz) δ7.15 (dd, J=3, 6 Hz, 1H), 8.64 (m, 1H), 9.15 (d, J=1.6 Hz, 1H).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05733912uspto-grants-1998_03