反应详情

A mixture of 1-(6-phenylpyridazin-3-yl)hydrazine (2.00 g, 10.7 mmol), glycolic acid (0.825 g, 10.8 mmol), p-TsOH.H2O (2.55 g, 13.4 mmol) in PhMe (50 mL) was refluxed for 14 h. PhMe was removed in vacuo. The resulting solids were diluted with water (30 mL). The mixture was brought to pH˜10 with 2N NaOH. The solids were isolated solid by filtration, washed with water and dried under vacuum to give an off white solid which was used without further purification. (ESI, pos. ion) m/z: 227.0 (M+H).

1. temperaturewas refluxed for 14 h
2. customPhMe was removed in vacuo
3. additionThe resulting solids were diluted with water (30 mL)
4. customThe solids were isolated solid
5. filtrationby filtration
6. washwashed with water
7. customdried under vacuum
8. customto give an off white solid which
9. customwas used without further purification