HRID34950

反应详情

EQUATION

反应方程式

HRID 34950 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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.

WORKUP

后处理

  1. temperaturecooled to 0°-5°
  2. distillationThe dimethylformamide was distilled off under reduced pressure
  3. dissolutionThe residue was dissolved in methylene chloride
  4. customseparated from the insoluble constituents
  5. customchromatographed on silica gel
  6. washelution agent