HRID1958296

反应详情

EQUATION

反应方程式

HRID 1958296 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

4-(5-Tributylstannanyl-[1,2,3]triazol-1-yl)-benzonitrile (0.15 g, 0.32 mmol), 6-bromo-N,5-dimethyl-3-oxo-4-[3-(trifluoromethyl)phenyl]-3,4-dihydropyrazine-2-carboxamide (SM2, 0.054 g, 0.14 mmol), Pd(PBut3)2 (10 mg) and DME (2 ml) were placed in a tube for microwave synthesis. The mixture was degassed with argon and heated in a synthesis microwave heater (CEM) at 100° C. (max 150 W) for 10 minutes. The solvent was removed in vacuo giving a crude product which was purified on silica and then further purified on preparative HPLC. The pure fractions were freeze-dried giving 27 mg (41%) of the title compound.

WORKUP

后处理

  1. customThe mixture was degassed with argon
  2. customThe solvent was removed in vacuo
  3. customgiving a crude product which
  4. customwas purified on silica
  5. customfurther purified on preparative HPLC
  6. customThe pure fractions were freeze-dried