HRID1160094

反应详情

EQUATION

反应方程式

HRID 1160094 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 4-amino-2,6-dichloro-5-nitropyrimidine, prepared as described in a), in methanol (30 ml), was added Raney nickel freshly prepared from 500 mg of alloy. The reaction mixture was stirred 20 hours in the hydrogen atmosphere. Then a new catalyst, prepared from 500 mg of alloy, was added and the reaction mixture was stirred next 24 hours in the hydrogen atmosphere. The catalyst was removed, the reaction mixture was concentrated in vacuo and the residue was extracted with hot water. Product, which was obtained after cooling of the water solution, was purified by chromatography (SiO2, VI—1:1)

WORKUP

后处理

  1. customfreshly prepared from 500 mg of alloy
  2. customThen a new catalyst, prepared from 500 mg of alloy
  3. additionwas added
  4. customThe catalyst was removed
  5. concentrationthe reaction mixture was concentrated in vacuo
  6. extractionthe residue was extracted with hot water
  7. customProduct, which was obtained
  8. customwas purified by chromatography (SiO2, VI—1:1)