HRID985516

反应详情

EQUATION

反应方程式

HRID 985516 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A suspension of 3-[3-(pyridin-3-yl)phenyl]imidazo[1,2-α]pyridin-7-ylmethanol (67 mg, 0.22 mmol) in 1,2-dichloroethane (5 ml) was treated with manganese(IV) oxide (0.19 g, 2.2 mmol) and the mixture heated at 50° C. for 18 h. The reaction was cooled to ambient temperature, diluted with 1,2-dichloroethane and pre-adsorbed onto silica. Purification by silica gel chromatography eluting with dichloromethane/methanol/conc. ammonia (95:5:0.5) gave the title compound (38 mg, 58%) as a yellow solid. 1H NMR (360 MHz, CDCl3) δH 7.36-7.45 (2H, m), 7.60-7.73 (3H, m), 7.76-7.78 (1H, m), 7.90-7.95 (1H, m), 7.97 (1H, s), 8.20 (1H, s), 8.40 (1H, d, J 7), 8.65 (1H, d, J 5), 8.90 (1H, s), 10.00 (1H, s); m/z (ES+) 300 (M++H).

WORKUP

后处理

  1. temperatureThe reaction was cooled to ambient temperature
  2. customPurification by silica gel chromatography
  3. washeluting with dichloromethane/methanol/conc