Реакция #94296

ord-044094b8de884a8a986cf92efd096934

Реагенты

Нет

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеthe exothermic reaction
  2. 2
    Другоеquenched
  3. 3
    Другоеon crushed ice
  4. 4
    workup.ADDITIONThe aqueous mixture is treated with sufficient 20% aqueous sodium hydroxide solution
  5. 5
    Другоеto provide a pH of 9-10
  6. 6
    Экстракцияthe liberated product extracted into chloroform (3 × 300 ml.)
  7. 7
    Сушкаdried over sodium sulfate
  8. 8
    Концентрированиеconcentrated to a light brown oil, 14.0 g

Методика

To 13.6 g. of 2-formamidomethylpyridine in a round-bottom flask is added 25 ml. of phosphorous oxychloride. Following the exothermic reaction, the reaction mixture is cooled to room temperature, and quenched on crushed ice. The aqueous mixture is treated with sufficient 20% aqueous sodium hydroxide solution to provide a pH of 9-10, and the liberated product extracted into chloroform (3 × 300 ml.). The extracts are combined, dried over sodium sulfate and concentrated to a light brown oil, 14.0 g.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04129567uspto-grants-1978_12