HRID1880380

反应详情

EQUATION

反应方程式

HRID 1880380 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
165 °C

PROCEDURE

实验过程

A microwave tube was charged with 5-bromo-7-chloro-3-methyl-1H-indazole (610 mg, 2.48 mmol), dioxane (5 mL), Hermann's catalyst (119 mg, 0.12 mmol) and a solution of sodium carbonate (790 mg, 7.46 mmol) in water (10 mL). The mixture was stirred for 20 sec, heated at 165° C. for 30 minutes in a microwave reactor at very high absorption setting. The reaction was vented before handling. The mixture was filtered through diatomaceous earth and washed with EtOAc. The filtrate was concentrated, the residue was dissolved in water and acidified to pH ˜3 with conc HCl. The solids were collected by filtration and dried to afford the title compound (420 mg, 82%).

WORKUP

后处理

  1. filtrationThe mixture was filtered through diatomaceous earth
  2. washwashed with EtOAc
  3. concentrationThe filtrate was concentrated
  4. dissolutionthe residue was dissolved in water
  5. filtrationThe solids were collected by filtration
  6. customdried