HRID550362

反应详情

EQUATION

反应方程式

HRID 550362 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

3-Amino-2-picolinic acid (4.14 g) was suspended in ethanol (100 ml) at room temperature with stirring. DMAP (3.7 g) was added and the reaction was stirred for 1 hour at room temperature. A further equivalent of DMAP (3.7 g) was added and the suspension disappeared, and then EDC (5.80 g) was added and the reaction was stirred at room temperature for 17 hours. The ethanol was evaporated to give a dark oil, water was added and the mixture was extracted with ethyl acetate, washed with brine and dried over magnesium sulphate. Evaporation of the solvent gave ethyl 3-amino-2-picolinate as a solid (6.5 g), mixed in a 2:1 ratio with DMAP.

WORKUP

后处理

  1. stirringthe reaction was stirred for 1 hour at room temperature
  2. stirringthe reaction was stirred at room temperature for 17 hours
  3. customThe ethanol was evaporated
  4. customto give a dark oil, water
  5. additionwas added
  6. extractionthe mixture was extracted with ethyl acetate
  7. washwashed with brine
  8. dry with materialdried over magnesium sulphate
  9. customEvaporation of the solvent