HRID530112

反应详情

EQUATION

反应方程式

HRID 530112 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
125 °C

PROCEDURE

实验过程

To a mixture of 2-chloro-7-methyl-5,8-diphenyl-7,8-dihydropteridin-6(5H)-one (175 mg, 0.5 mmol), 5-aminoindazole (99 mg, 0.75 mmol), in trifluoroethanol (2 mL) in a microwave reactor vial was added trifluoroacetic acid (171 mg). The vial was then sealed and heated in a microwave reactor at 125° C. for 30 minutes. The reaction mixture was then diluted with ethyl acetate (25 mL) and washed with aqueous saturated aq. sodium bicarbonate. The organic layer was dried (Na2SO4) and evaporated to give a crude material, which was then purified by silica gel column chromatography (eluent: 2% methanol in dichloromethane) to give the desired product (40%).

WORKUP

后处理

  1. customThe vial was then sealed
  2. washwashed with aqueous saturated aq. sodium bicarbonate
  3. dry with materialThe organic layer was dried (Na2SO4)
  4. customevaporated
  5. customto give a crude material, which
  6. customwas then purified by silica gel column chromatography (eluent: 2% methanol in dichloromethane)