HRID440871

反应详情

EQUATION

反应方程式

HRID 440871 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

248.2 g (0.96 mol) of 2-methyl-5-nitrophenylguanidine nitrate are added to a solution of 170 g (0.96 mol) of 3-dimethylamino-1-(3-pyridyl)-2-propen-1-one in 2.0 liters of isopropanol. After the addition of 42.5 g of sodium hydroxide, the reddish suspension is boiled at reflux for 12 hours. After cooling to 0°, filtration, washing with 2.0 liters of isopropanol and 3×400 ml of methanol and drying, there is obtained N-(2-methyl-5-nitrophenyl)-4-(3-pyridyl)-2-pyrimidine-amine, m.p. 195°-198°, Rf =0.68 (methylene chloride:methanol=9.1).

WORKUP

后处理

  1. temperatureat reflux for 12 hours
  2. temperatureAfter cooling to 0°
  3. filtrationfiltration
  4. washwashing with 2.0 liters of isopropanol and 3×400 ml of methanol
  5. customdrying