HRID1681048

反应详情

EQUATION

反应方程式

HRID 1681048 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

17.7 g (0.256 moles) of sodium nitrate are added to a solution of 39.5 g (0.233 mole) of 6-amino-2-(ethoxymethyl)-4(3H)-pyrimidinone in 336 ml (0.336 mole) of 1 N sodium hydroxide. A solution of 17.9 ml (0.320 mole) of 96% sulphuric acid diluted in 179 ml of water is then added dropwise at between 0° and 5° C. The precipitate formed is isolated by filtration immediately after completion of the addition. The solid obtained is washed with cold water and then with ethyl ether. After drying, it is used in the next step without further purification. Yld: 46.2 (quantitative), m.p. 163°-165° C. An analytical sample was obtained by recrystallization from methanol.

WORKUP

后处理

  1. additionis then added dropwise at between 0° and 5° C
  2. customThe precipitate formed
  3. customis isolated by filtration
  4. additionimmediately after completion of the addition
  5. customThe solid obtained
  6. washis washed with cold water
  7. customAfter drying
  8. customit is used in the next step without further purification
  9. customAn analytical sample was obtained by recrystallization from methanol