HRID244735

反应详情

EQUATION

反应方程式

HRID 244735 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

5-Isoquinolinylboronic acid (21 mg), 0.6M potassium carbonate solution (200 μl) and Pd(dppf)Cl2 (10 mg) in 1,4-dioxane (1 ml) were treated with a solution of N-(6-bromo-1H-indazol-4-yl)-2-methyl-1,3-thiazole-4-carboxamide (40 mg) in 1,4-dioxane (1 ml). The reaction vessel was sealed and heated under microwave irradiation at 150° C. for 30 min. After cooling the solvent was removed in vacuo. The sample was redissolved in methanol and loaded onto C18 reverse phase SPE (0.5 g). Product was eluted with acetonitrile/TFA (0.1%) (3×3 ml), and concentrated under a stream of nitrogen using blow down apparatus. Purification by mass directed preparative HPLC (Method C) gave the title compound.

WORKUP

后处理

  1. customThe reaction vessel was sealed
  2. temperatureAfter cooling the solvent
  3. customwas removed in vacuo
  4. dissolutionThe sample was redissolved in methanol
  5. washProduct was eluted with acetonitrile/TFA (0.1%) (3×3 ml)
  6. concentrationconcentrated under a stream of nitrogen using blow down apparatus
  7. customPurification by mass