HRID606005

反应详情

EQUATION

反应方程式

HRID 606005 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

150 mg of 6-bromo-2-phenylimidazo[1,2-a]pyridine, 125 mg of 4-(hydroxymethyl)phenylboronic acid, 19 mg of tetrakis(triphenylphosphine)palladium and 2 ml of acetonitrile are placed in a microwave tube. Under a stream of nitrogen, 2 ml of nitrogen-degassed toluene and then 2 ml of a 2M solution of sodium carbonate are added thereto. The tube is placed in a microwave device and irradiated at 150° C. for 15 min. The organic phase is recovered, dried and then concentrated under reduced pressure. The residue is taken up with diisopropyl ether and the precipitate is recovered by filtration, washed and dried. It is purified by recrystallization from n-butanol. 52 mg of compound are obtained. Mp=238-240° C. 1H NMR (DMSO-d6, δ in ppm): 4.54 (d, J=5.5 Hz, 2H); 5.2 (t, J=5.6 Hz, 1H); from 7.24 to 7.73 (m, 9H); 7.96 (m, 2H); 8.36 (s, 1H); 8.84 (t, J=1.3 Hz, 1H). M+H=301.

WORKUP

后处理

  1. customUnder a stream of nitrogen, 2 ml of nitrogen-degassed toluene
  2. addition2 ml of a 2M solution of sodium carbonate are added
  3. customirradiated at 150° C. for 15 min
  4. customThe organic phase is recovered
  5. customdried
  6. concentrationconcentrated under reduced pressure
  7. filtrationthe precipitate is recovered by filtration
  8. washwashed
  9. customdried
  10. customIt is purified by recrystallization from n-butanol