反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of (2-(5-bromo-2-chloropyridin-3-yl)imidazo[1,2-a]pyridin-3-yl)methanol (20 mg, 0.06 mmol) in DMF (2 mL), K2CO3 (20 mg, 0.14 mmol) was stirred at 100° C. overnight. The reaction mixture was concentrated in vacuo. The resulting residue was suspended with water and extracted with EtOAc. The combined organic phases were washed with brine, dried over Na2SO4, filtered and concentrated in vacuo. The crude product was purified using PTLC (eluted with dichloromethane:MeOH=50:1) to provide 2-bromo-4-aza-6H-chromeno[4′,3′:4,5]imidazo[1,2-a]pyridine (7 mg, yield: 39%). 1H-NMR (CDCl3, 400 MHz) δ 8.23 (d, J=2.4 Hz, 1H), 8.13 (d, J=2.4 Hz, 1H), 7.75 (d, J=6.8 Hz, 1H), 7.66 (d, J=9.2 Hz, 1H), 7.27˜7.30 (m, 1H), 6.90˜6.95 (m, 1H), 5.93 (s, 2H). MS (M+H)+: 302/304.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated in vacuo
- extractionextracted with EtOAc
- washThe combined organic phases were washed with brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe crude product was purified
- washPTLC (eluted with dichloromethane:MeOH=50:1)