HRID1896518

反应详情

EQUATION

反应方程式

HRID 1896518 的结构方程式

CONDITIONS

反应条件

温度
160 °C

PROCEDURE

实验过程

A mixture of 1-chloro-5H-pyrido[4,3-b]indole-4-carboxamide in conc. NH4OH (0.07 M) was heated in a microwave reactor at 160° C. for 1 h in a sealed tube. The reaction mixture was cooled to room temperature and partitioned between THF/EtOAc and saturated NaHCO3. After separation of the organic phase, the aqueous phase was extracted again with THF/EtOAc, and the combined organic phases were washed with brine, dried over Na2SO4 and filtered. After evaporation of the organic solvents, the residue was purified by flash chromatography (0-10% MeOH in EtOAc) to provide the title compound as an off-white solid.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. custompartitioned between THF/EtOAc and saturated NaHCO3
  3. customAfter separation of the organic phase
  4. extractionthe aqueous phase was extracted again with THF/EtOAc
  5. washthe combined organic phases were washed with brine
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. customAfter evaporation of the organic solvents
  9. customthe residue was purified by flash chromatography (0-10% MeOH in EtOAc)