反应详情

温度

90 °C

A solution of sodium nitrite (140 mg, 2 mmol) in H2O (1 ml) was added to a stirred solution of 3-imidazo[1,2-a]pyridin-3-yl-phenylamine (420 mg, 2 mmol) in 2N HCl (4 ml) such that the internal temperature <5° C. After complete addition the reaction was stirred 15 minutes at this temperature before the addition of aminoacetonitrile hydrogen sulphate (310 mg, 2 mmol) in H2O (1 ml) [internal temperature maintained <5° C.]. After 1 hour NaOAc (7 g) was added. The mixture was stirred for 1 hour with ice bath cooling, then the solid was collected by filtration. This material was taken up in EtOH directly (˜10 ml). This solution was stirred and heated at 90° C. for 18 hours under N2. After cooling to RT the volatiles were removed in vacuo and the residue was purified by chromatography on silica (100% CH2Cl2→4% 2M NH3-MeOH/CH2Cl2) to give the title compound (219 mg, solid). MS: [M+H]+ 277

1. additionAfter complete addition the reaction
2. temperaturecooling
3. filtrationthe solid was collected by filtration
4. stirringThis solution was stirred
5. temperatureAfter cooling to RT the volatiles
6. customwere removed in vacuo
7. customthe residue was purified by chromatography on silica (100% CH2Cl2→4% 2M NH3-MeOH/CH2Cl2)