HRID2401223

反应详情

EQUATION

反应方程式

HRID 2401223 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of [6-(methylsulfinyl)-4-pyrimidinyl]acetonitrile (Intermediate 16, 150 mg, 0.828 mmol) and 1-[2-(trifluoromethyl)-1H-pyrrolo[2,3-b]pyridin-5-yl]methanamine (Intermediate 5, 178 mg, 0.828 mmol) in isopropanol (7 mL) was stirred and heated at 80° C. overnight. The reaction mixture was cooled to room temperature and condensed. This solid was dissolved in a mixture of acetonitrile and DMSO (1:1) (2.7 mL) and purified by MDAP (3 injections). Fractions containing the suspected product were combined and concentrated under reduced pressure. The solid was dissolved in a mixture of acetonitrile and DMSO (1:1) (1.8 mL) and purified again by MDAP (2 injections). Fractions containing the suspected product were combined and concentrated under reduced pressure to give the title compound as a solid (23 mg);

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customcondensed
  3. custompurified by MDAP (3 injections)
  4. additionFractions containing the suspected product
  5. concentrationconcentrated under reduced pressure
  6. dissolutionThe solid was dissolved in a mixture of acetonitrile and DMSO (1:1) (1.8 mL)
  7. custompurified again by MDAP (2 injections)
  8. additionFractions containing the suspected product
  9. concentrationconcentrated under reduced pressure