反应详情

温度

100 °C

A mixture of 5-(4-chloro-phenyl)-pyrazolo[1,5-a]pyrimidine-7-ol (4.8 g, 19.5 mmol), phosphorous oxychloride (7.2 mL, 78 mmol), and N,N-dimethylaniline (0.87 mL, 7.0 mmol) was stirred at 100° C. for 2 h. The mixture was evaporated in vacuo and the residue was partitioned between water and dichloromethane. The organic phase was washed with water, dried (Na2SO4), and evaporated in vacuo. The remaining solid was crystallized from EtOAc to give 7-chloro-5-(4-chloro-phenyl)-pyrazolo[1,5-a]pyrimidine (3.50 g, 66%) as a yellow solid; mp 151-153° C.

1. customThe mixture was evaporated in vacuo
2. customthe residue was partitioned between water and dichloromethane
3. washThe organic phase was washed with water
4. dry with materialdried (Na2SO4)
5. customevaporated in vacuo
6. customThe remaining solid was crystallized from EtOAc