Реакция #63228

ord-73ec8076ef72413595d304b362e40316

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураcooled to 0°-5°
  2. 2
    workup.DISTILLATIONThe dimethylformamide was distilled off under reduced pressure
  3. 3
    workup.DISSOLUTIONThe residue was dissolved in methylene chloride
  4. 4
    Другоеseparated from the insoluble constituents
  5. 5
    Другоеchromatographed on silica gel
  6. 6
    Промывкаelution agent

Методика

15.4 ml of ethanolamine were placed under argon with 30 ml of dimethylformamide and cooled to 0°-5°. A solution of 11.3 g of picolinic acid chloride in 100 ml of dimethylformamide was added dropwise thereto at 0°-10° and the mixture was stirred at room temperature overnight. The dimethylformamide was distilled off under reduced pressure. The residue was dissolved in methylene chloride and separated from the insoluble constituents, and thereafter chromatographed on silica gel; elution agent: methylene chloride, thereafter methylene chloride/methanol (9:1). N-(2-Hydroxyethyl)pyridine-2-carboxamide was obtained as a yellow oil.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04764522uspto-grants-1988_08