HRID859108

反应详情

EQUATION

反应方程式

HRID 859108 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-4-pyridyl)-2-propen-1-one (2.22 g, 10.5 mmol), 3-methoxy-phenyl-guanidine nitrite (2.40 g, 10.5 mmol), lithium hydroxide (350 mg, 14.5 mmol) in 2-butanol (25 mL) is heated to reflux for 8 hours. The reaction mixture is cooled to room temperature, concentrated and water (60 mL) is added. The resultant solid is collected by filtration and washed with water, isopropanol and dried to give N-[3-methoxy-phenyl]-4-(2-chloro-4-pyridyl)-2-pyrimidineamine (2.81 g); ESI-MS (m/z): 313 (M++H).

WORKUP

后处理

  1. temperatureis heated
  2. temperatureto reflux for 8 hours
  3. concentrationconcentrated
  4. additionwater (60 mL) is added
  5. filtrationThe resultant solid is collected by filtration
  6. washwashed with water, isopropanol
  7. customdried