HRID1288284

反应详情

EQUATION

反应方程式

HRID 1288284 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a stirred solution of sodium (1.15 g.) in dry ethanol (20 ml.) was added ethyl cyanoacetate (1.8 ml.) followed after 15 minutes by isobutyramidine sulphate (2.25 g.). The mixture was refluxed for 20 hours, evaporated to dryness, the residue triturated with water (30 ml.) and the pH adjusted to 6 by the addition of hydrochloric acid. After cooling to 0° C, 4-amino-2-isopropylpyrimid-6-one (1.7 g.), m.p. 248°-250° C, was filtered off and recrystallised from ethanol to give 4-amino-2-isopropylpyrimid-6-one (0.95 g.), m.p. 254° C.

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 20 hours
  2. customevaporated to dryness
  3. customthe residue triturated with water (30 ml.)
  4. additionthe pH adjusted to 6 by the addition of hydrochloric acid
  5. filtration4-amino-2-isopropylpyrimid-6-one (1.7 g.), m.p. 248°-250° C, was filtered off
  6. customrecrystallised from ethanol