HRID1094519

反应详情

EQUATION

反应方程式

HRID 1094519 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

2.9 g (12 mMol) 5-tert-butyl-2-(4-methoxy-phenyl)-2H-pyrazol-3-ylamine and 3.8 g (12 mMol) 6-(6-chloropyrimidin-4-yloxy)-naphthalene-1-carbonyl chloride (described under Step 19.3) are dissolved in 10 ml CH2Cl2 and cooled to 0° C. 0.99 ml (12 mMol) Pyridine are added dropwise and after complete addition the reaction is allowed to warm to rt. It is stirred for 2 h at ambient temperature. The reaction is worked up by addition of 150 ml CH2Cl2 and aq. extraction with sat. Na2CO3 solution. The organic layer is subsequently washed with brine and dried. After removal of the solvents the remaining crude product is purified by flash chromatography (SiO2; hexanes/EtOAc, gradient 3:1 to 2:1) to give the title compound as a yellow solid: m.p.: 163-164° C.

WORKUP

后处理

  1. additionafter complete addition the reaction
  2. temperatureto warm to rt
  3. washThe organic layer is subsequently washed with brine
  4. customdried
  5. customAfter removal of the solvents the remaining crude product
  6. customis purified by flash chromatography (SiO2; hexanes/EtOAc, gradient 3:1 to 2:1)