HRID1896518
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperatureThe reaction mixture was cooled to room temperature
- custompartitioned between THF/EtOAc and saturated NaHCO3
- customAfter separation of the organic phase
- extractionthe aqueous phase was extracted again with THF/EtOAc
- washthe combined organic phases were washed with brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- customAfter evaporation of the organic solvents
- customthe residue was purified by flash chromatography (0-10% MeOH in EtOAc)