HRID2240272

反应详情

EQUATION

反应方程式

HRID 2240272 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

82 mg (0.31 mmol) of 4-(4-amino-2-fluorobenzyl)-1H-pyrrolo[2,3-b]pyridine-3-carbonitrile and 67 mg (0.34 mmol) of 4-chloro-6-trifluoromethylpyrimidine-2-amine are suspended in 3 ml of water, 1.5 ml of ethanol and 0.15 ml of 4N hydrochloric acid. The reaction mixture is heated at reflux for 2 hours. After cooling, the mixture is made alkaline using dilute aqueous sodium hydroxide solution, a little methanol is added, the mixture is extracted with ethyl acetate and the solvent is removed under reduced pressure. The residue is purified by preparative HPLC. This gives crystals.

WORKUP

后处理

  1. temperatureThe reaction mixture is heated
  2. temperatureat reflux for 2 hours
  3. temperatureAfter cooling
  4. extractionthe mixture is extracted with ethyl acetate
  5. customthe solvent is removed under reduced pressure
  6. customThe residue is purified by preparative HPLC