HRID1641393

反应详情

EQUATION

反应方程式

HRID 1641393 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

To a solution of 2,5,6-trichloro-N-(5-methyl-1H-pyrazol-3-yl)pyrimidin-4-amine (Method 39; 2.0 g, 8.2 mmol) in absolute EtOH (40 ml) were added DIEA (2.5 ml) and (15)-1-(5-fluoropyridin-2-yl)ethanamine (Method 6; 1.2 g, 8.2 mmol) and the resulting solution was heated to 140° C. for 12 hours. The mixture was partitioned between EtOAc and H2O, the organic layer was washed with brine and dried. The solvents were removed under reduced pressure to give an oil which was purified by Gilson (20-75% acetonitrile/H2O, 35 min) to give the titled compound as solid (762 mg). m/z: 383.

WORKUP

后处理

  1. customThe mixture was partitioned between EtOAc and H2O
  2. washthe organic layer was washed with brine
  3. customdried
  4. customThe solvents were removed under reduced pressure
  5. customto give an oil which
  6. customwas purified by Gilson (20-75% acetonitrile/H2O, 35 min)