HRID913299

反应详情

EQUATION

反应方程式

HRID 913299 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a solution of 4-(2-chloro-4-pyrimidinyl)-N-(3-fluorophenyl)-2-pyridinamine (i.e., the product of Step C) (55 mg, 0.18 mmol) in toluene (3.0 mL) was added 2-methoxy-1-aminopropane hydrochloride (125 mg, 1.0 mmol) and potassium carbonate (200 mg, 1.5 mmol). The mixture was stirred at 100° C. for 2 h and then allowed to cool to room temperature. The mixture was partitioned with water and ethyl acetate and the water layer was decanted. The organic layer was washed with brine and passed through a Celite® containing drying tube. The solvent was evaporated, and the resulting residue was chromatographed using 5% to 60% ethyl acetate in hexanes as eluant to give an oil which solidified upon standing. This solid was suspended in hexanes, filtered and washed with hexanes to give 25 mg of the title compound as a yellow solid, m.p. 103-105° C.

WORKUP

后处理

  1. temperatureto cool to room temperature
  2. customThe mixture was partitioned with water and ethyl acetate
  3. customthe water layer was decanted
  4. washThe organic layer was washed with brine
  5. additioncontaining
  6. customdrying tube
  7. customThe solvent was evaporated
  8. customthe resulting residue was chromatographed
  9. customto give an oil which
  10. filtrationfiltered
  11. washwashed with hexanes