HRID37466

反应详情

EQUATION

反应方程式

HRID 37466 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

In a mixture of 90 ml of 2% hydrochloric acid and 60 ml of dioxane was dissolved 3.50 g (10 mmol) of 2-amino-3,4-diethoxycarbonyl-6-phenylpyridine hydrochloride. A solution of 0.83 g (1.2 eq.) of sodium nitrite dissolved in 3 ml of water was added dropwise thereto. The mixture was stirred at room temperature for 4 hours and left standing overnight. The solvent was distilled off. The resulting crystals were collected by filtration with water. The crystals were recrystallized from ethanol, to give pale yellow prisms.

WORKUP

后处理

  1. additionwas added dropwise
  2. waitleft
  3. waitstanding overnight
  4. distillationThe solvent was distilled off
  5. filtrationThe resulting crystals were collected by filtration with water
  6. customThe crystals were recrystallized from ethanol
  7. customto give pale yellow prisms