HRID66021

反应详情

EQUATION

反应方程式

HRID 66021 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 47 g. of 2-aminopyridine, 120 g. of 45% chloroacetaldehyde solution in water and 50.4 g. of sodium bicarbonate in 400 ml. of anhydrous ethanol and 100 ml. of water is heated to reflux for 3 hrs. The reaction mixture is cooled, treated with 900 ml. of water and extracted with diethyl ether (3 × 700 ml.). The combined extracts are dried over sodium sulfate and concentrated to a brown oil. Distillation gives 18.8 g. of the desired intermediate as a light yellow oil, b.p. 70° C./0.02 mm.

WORKUP

后处理

  1. additionA mixture of 47 g
  2. temperatureto reflux for 3 hrs
  3. temperatureThe reaction mixture is cooled
  4. additiontreated with 900 ml
  5. extractionof water and extracted with diethyl ether (3 × 700 ml.)
  6. dry with materialThe combined extracts are dried over sodium sulfate
  7. concentrationconcentrated to a brown oil
  8. distillationDistillation
  9. customgives 18.8 g