反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of N-(3-chlorophenyl)-1-methyl-7-(4-thiomorpholinylcarbonyl)-1H-pyrrolo[3,2-c]pyridin-4-amine (100 mg) in DCM (3 ml) was cooled to −78 C and meta-chloroperoxybenzoic acid (58 mg) was added and the reaction stirred under argon for 30 minutes. The reaction was partitioned between dichloromethane and water and the organic layer separated. The organic layer was then washed three times with water, aqueous sodium sulfite solution, dried (Na2SO4) and evaporated. The residue was purified by MDAP to afford the free base as a white solid (84 mg). This was dissolved in methanol and a solution of 11.0M hydrochloric acid in diethyl ether (0.5 ml) and after evaporation afforded the title compound as a white solid (85 mg).
WORKUP
后处理
- additionwas added
- customThe reaction was partitioned between dichloromethane and water
- customthe organic layer separated
- washThe organic layer was then washed three times with water, aqueous sodium sulfite solution
- dry with materialdried (Na2SO4)
- customevaporated
- customThe residue was purified by MDAP