反应详情

温度

-78 °C

A solution of 1,5-dimethyltetrazole (20 g; 0.204 mole) in dry THF (200 mL) was cooled to -78° C. and treated with n-butyllithium (91 mL of 2.5 molar solution in hexane; 0.227 mole) and the mixture stirred at -78° C. for 30 minutes. Benzophenone (31.1 g; 0.171 mole) was added and the mixture stirred at -78° C. for 30 minutes and allowed to warm up to 23° C. and stirred for 15 hours. The mixture was quenched with 2N HCl (100 mL) and extracted with EtOAc (3×150 mL). The combined organic layers were dried (MgSO4) and evaporated. The residue was crystallized from EtOAc-Hexane to afford the title compound as a white solid (10.5 g; 22%); m.p.=175°-176° C. (crystallized from EtOAc-hexane). MS (CI): m/e=281 for (M+H)+.

1. stirringthe mixture stirred at -78° C. for 30 minutes
2. temperatureto warm up to 23° C.
3. stirringstirred for 15 hours
4. customThe mixture was quenched with 2N HCl (100 mL)
5. extractionextracted with EtOAc (3×150 mL)
6. dry with materialThe combined organic layers were dried (MgSO4)
7. customevaporated
8. customThe residue was crystallized from EtOAc-Hexane