HRID513589
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
Sat. NH4Cl (0.49 g, 9.09 mmol) was added to a solution of 3-nitro-pyridine-2-sulfonic acid quinolin-8-ylamide (Intermediate 259) (0.3 g, 0.91 mmol) in MeOH:THF(10 ml, 1:1) followed by zinc powder (0.48 g, 7.27 mmol) and the mixture was stirred at room temperature for 18 h. The mixture was filtered through celite and washed with THF. The filtrate was concentrated in vacuo and the residue was diluted with EtOAc. The organic phase was dried (Na2SO4) and concentrated in vacuo. The crude residue was purified by column chromatography with DCM/MeOH as the eluent to give the title compound (0.26 g, 95%)
WORKUP
后处理
- filtrationThe mixture was filtered through celite
- washwashed with THF
- concentrationThe filtrate was concentrated in vacuo
- additionthe residue was diluted with EtOAc
- dry with materialThe organic phase was dried (Na2SO4)
- concentrationconcentrated in vacuo
- customThe crude residue was purified by column chromatography with DCM/MeOH as the eluent