HRID16456

反应详情

EQUATION

反应方程式

HRID 16456 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

52 mg (0.14 mmol) of 6-chloro-N4-[3-fluoro-4-(1H-pyrrolo[2,3-b]pyridin-4-yloxy)-phenyl]pyrimidine-2,4-diamine (from example 60) are dissolved in 2.5 ml of 2-ethylhexanol. 0.24 ml of N-ethyldiisopropylamine and 36 mg (0.42 mmol) of morpholine are added, and the mixture is heated at 150° C. bath temperature for 20 hours. After cooling, a little DMF is added and the mixture is chromatographed on silica gel 60 (gradient column: mobile phase: DCM:methanol=50:1, then 3:1). This gives an oil which is purified by preparative HPLC.

WORKUP

后处理

  1. temperatureAfter cooling
  2. customthe mixture is chromatographed on silica gel 60 (gradient column
  3. customThis gives an oil which
  4. customis purified by preparative HPLC