HRID1776896

反应详情

EQUATION

反应方程式

HRID 1776896 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. extractionextracted with EtOAc
  3. washThe combined organic phases were washed with brine
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe crude product was purified
  8. washPTLC (eluted with dichloromethane:MeOH=50:1)