HRID859109

反应详情

EQUATION

反应方程式

HRID 859109 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3-dimethylamino-1-(2-chloro-3-pyridyl)-2-propen-1-one (3.50 g, 16.5 mmol), 3-methoxy-phenyl-guanidine nitrite (3.70 g, 16.2 mmol), lithium hydroxide (412 mg, 16.5 mmol) in 2-butanol (15 mL) is heated to reflux overnight. The reaction mixture is cooled to room temperature, concentrated and water (60 mL) is added. The resultant solid is filtered, washed with water, isopropanol and dried to give N-[3-methoxy-phenyl]-4-(2-chloro-3-pyridyl)-2-pyrimidineamine (3.95 g); ESI-MS (m/z): 313 (M++H).

WORKUP

后处理

  1. temperatureis heated
  2. temperatureto reflux overnight
  3. concentrationconcentrated
  4. additionwater (60 mL) is added
  5. filtrationThe resultant solid is filtered
  6. washwashed with water, isopropanol
  7. customdried