HRID1094523

反应详情

EQUATION

反应方程式

HRID 1094523 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

100 mg (0.19 mMol) 6-(6-Chloro-pyrimidin-4-yloxy)-naphthalene-1-carboxylic acid [5-tert-butyl-2-(4-fluoro-phenyl)-2H-pyrazol-3-yl]-amide (Step 20.1) and 73 μl (0.42 mMol) 1-(3-aminopropyl)-4-methylpiperazine are dissolved in 5 ml EtOH. The reaction mixture is stirred at reflux for 30 h. It is worked up by removal of all volatiles under reduced pressure. The remaining crude product is purified by flash chromatography (combi-flash: 14 g column, CH2Cl2/MeOH; gradient 0-20% MeOH) to give the title compound as a yellow solid: m.p.: 131-133° C.

WORKUP

后处理

  1. temperatureat reflux for 30 h
  2. customIt is worked up by removal of all volatiles under reduced pressure
  3. customThe remaining crude product is purified by flash chromatography (combi-flash: 14 g column, CH2Cl2/MeOH; gradient 0-20% MeOH)