HRID440869

反应详情

EQUATION

反应方程式

HRID 440869 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.38 g (5.68 mmol) of 3-nitrophenyl-guanidine nitrate and 0.25 g (6.24 mmol) of sodium hydroxide are added to a solution of 1 g (5.68 mmol) of 3-dimethylamino-1-(4-pyridyl)-2-propen-1-one [U.S. Pat. No. 4,281,000] in 8 ml of isopropanol. The yellow suspension is heated at reflux for 20 hours and then cooled to 0°. After washing with 30 ml of isopropanol the filtration residue is made into a slurry in succession in 15 ml of ethanol and then in 15 ml of water and filtered each time. Drying under HV yields N-(3-nitrophenyl)-4-(4-pyridyl)-2-pyrimidine-amine; m.p. 282°-284°.

WORKUP

后处理

  1. temperatureThe yellow suspension is heated
  2. temperatureat reflux for 20 hours
  3. temperaturecooled to 0°
  4. washAfter washing with 30 ml of isopropanol the filtration residue
  5. filtrationin 15 ml of water and filtered each time
  6. customDrying under HV