HRID908247

反应详情

EQUATION

反应方程式

HRID 908247 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a MeOH 25 mL solution of tert-butyl[(6-bromo-3H-imidazo[4,5-b]pyridin-2-yl)methyl]carbamate (Priepke, H.; Pfau, R; Gerlach, K.; Gillard, J.; Bauer, E.; Wienen, E.; Wolfgang, H.; Sandra N. H. WO 2004056784, 2004.) (1.2 g, 3.66 mmol) were added Et3N (1.11 g, 11 mmol), Pd(dppf)Cl2 (263 mg, 0.366 mmol). The reaction mixture was stirred at 80° C. under CO atmosphere (50 psi) for 24 hr. The reaction mixture was cooled to room temperature, filtered and the filtrate was concentrated, chromatographed on silica gel eluting with DCM: MeOH: TEA (50:1:0.01, v/v/v) to give the title compound (0.9 g, 82%).

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. filtrationfiltered
  3. concentrationthe filtrate was concentrated
  4. customchromatographed on silica gel eluting with DCM: MeOH: TEA (50:1:0.01, v/v/v)