反应详情

温度

75 °C

A solution of 2-bromo-5-fluoro-3-nitropyridine (1.176 g, 5.321 mmol) in 2M NH3 in MeOH (20 ml) was sealed in an autoclave and then heated at 75° C. for 6 h and then at 90° C. for a further 18 h. The reaction mixture was then cooled and evaporated, treated with sat. aq. NaHCO3 (100 ml) and then extracted with 5% MeOH/DCM (3×200 ml). The combined organic phases were dried and the solvent was removed. The residue was subjected to column chromatography on silica gel using a 0-5% MeOH in DCM gradient to provide the desired compound as a yellow solid (561 mg, 67%).

1. temperatureThe reaction mixture was then cooled
2. customevaporated
3. additiontreated with sat. aq. NaHCO3 (100 ml)
4. extractionextracted with 5% MeOH/DCM (3×200 ml)
5. customThe combined organic phases were dried
6. customthe solvent was removed