반응 #63228

ord-73ec8076ef72413595d304b362e40316

반응 방정식

NCCO
ethanolamine
O=C(Cl)c1ccccn1
picolinic acid chloride
O=C(NCCO)c1ccccn1
N-(2-Hydroxyethyl)pyridine-2-carboxamide

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도cooled 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
    기타separated from the insoluble constituents
  5. 5
    기타chromatographed on silica gel
  6. 6
    세척elution agent

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04764522uspto-grants-1988_08