Реакция #65752

ord-133574a6edea4a3e8e8cf537230a23b2

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONwas added dropwise to the solution
  2. 2
    workup.WAITleft
  3. 3
    Другоеstanding in a refrigerator overnight
  4. 4
    ФильтрацияThe resulting crystals were collected by filtration
  5. 5
    ДругоеThe crystals were recrystallized from ethyl acetate
  6. 6
    Другоеto give colorless plates

Методика

In 90 ml of 2% hydrochloric acid was dissolved 2.52 g (10 mmol) of 2-amino-3,4-diethoxycarbonyl-6-methylpyridine. A solution of 0.83 g (1.2 eq.) of sodium nitrite dissolved in 3 ml of water was added dropwise to the solution. The mixture was stirred at room temperature for 1 hour and left standing in a refrigerator overnight. The resulting crystals were collected by filtration. The crystals were recrystallized from ethyl acetate to give colorless plates.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05420275uspto-grants-1995_05