HRID1995350

反应详情

EQUATION

反应方程式

HRID 1995350 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1.06 g of 4-methyl-2-pyridinecarboxylic acid, 1.28 g of N,N'-carbonyldiimidazole, 25 ml of dimethylformamide and 12 ml of tetrahydrofuran is stirred at room temperature for 3 hours. 0.72 g of 5-aminotetrazole is added to the mixture and said mixture is stirred at 80° C. for 3 hours. Then, the reaction mixture is concentrated under reduced pressure to remove solvent. Water is added to the residue, and the aqueous mixture is adjusted to pH 2 with 10% hydrochloric acid. The crystalline precipitates are collected by filtration, washed with water and then recrystallized from a mixture of dimethylformamide and water. 0.52 g of N-(5-tetrazolyl)-4-methyl-2-pyridinecarboxamide is thereby obtained.

WORKUP

后处理

  1. stirringis stirred at 80° C. for 3 hours
  2. concentrationThen, the reaction mixture is concentrated under reduced pressure
  3. customto remove solvent
  4. additionWater is added to the residue
  5. customThe crystalline precipitates
  6. filtrationare collected by filtration
  7. washwashed with water
  8. customrecrystallized from a mixture of dimethylformamide and water