HRID2409051
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 mixture of 6-(1-ethoxyvinyl)-3-(4-methoxybenzyl)-3H-imidazo[4,5-c]pyridine (440 mg, 1.42 mmol) in MeOH (2 mL) was added an aqueous solution of HCl (1N, 0.5 mL) and stirred at RT for 30 min. To the reaction mixture was added an aqueous ammonia solution (35%) until the pH was approximately 8. The aqueous solution was extracted with EtOAc (50 mL×3). The combined extracts were washed with water and brine, dried (MgSO4), filtered, and concentrated under reduced pressure. The residue was purified by SiO2 chromatography eluting with petroleum ether:EtOAc (1:1) to afford 300 mg (75%) of 1-(3-(4-methoxybenzyl)-3H-imidazo[4,5-c]pyridin-6-yl)ethanone as a white solid. MS (ESI): m/z=282.3 [M+1]+.
WORKUP
后处理
- extractionThe aqueous solution was extracted with EtOAc (50 mL×3)
- washThe combined extracts were washed with water and brine
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe residue was purified by SiO2 chromatography
- washeluting with petroleum ether:EtOAc (1:1)