HRID42253

反应详情

EQUATION

反应方程式

HRID 42253 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A mixture of 6-(1H-indol-4-yl)-1H-indazol-4-amine (500 mg, 2.014 mmol), 2-benzofuran-1,3-dione (298 mg, 2.014 mmol) and DMF (2.5 ml) was placed in a Biotage vial (2-5 ml) equipped with a magnetic stirrer bar. The vial was placed in a Biotage Initiator microwave and heated at 150° C. for 30 min then again at 150° C. for a further 15 min. The reaction mixture was evaporated to dryness to give a brown oil which was dissolved in dichloromethane and applied to a 100 g silica SPE cartridge. The cartridge was eluted on a Flashmaster (II) instrument using a gradient of 0-100% ethyl acetate in cyclohexane over 40 min followed by 0-20% methanol in cyclohexane over 15 min. Appropriate fractions were combined and evaporated to give the title compound (481 mg) as a pale yellow foam.

WORKUP

后处理

  1. customequipped with a magnetic stirrer bar
  2. customThe reaction mixture was evaporated to dryness
  3. customto give a brown oil which
  4. washThe cartridge was eluted on a Flashmaster (II) instrument
  5. customover 40 min
  6. waitfollowed by 0-20% methanol in cyclohexane over 15 min
  7. customevaporated