反应详情

温度

50 °C

6-(2-Methylpyridin-3-yloxy)-pyridazine-3-carboxylic acid ethyl ester (D11) (1.07 g, 4.13 mmol) and hydrazine monohydrate (0.23 ml, 7.22 mmol) in ethanol (100 ml) was stirred at room temperature for 1 hour then heated at 50° C. for 1 hour and finally heated at reflux for 4 hours. A second portion of hydrazine monohydrate (0.23 ml, 7.22 mmol) was added and the mixture refluxed for a further 2 hours. After being allowed to cool the solvent was removed in vacuo. The off-white solid residue was subjected to column chromatography using 25% MeOH/EtOAc as eluant, resulting in a white crystalline product (0.63 g, 62%).

1. temperaturefinally heated
2. temperatureat reflux for 4 hours
3. temperaturethe mixture refluxed for a further 2 hours
4. temperatureto cool the solvent
5. customwas removed in vacuo