反应详情

温度

-78 °C

A solution of 1,5-dimethyltetrazole (29.25 g; 0.298 mole) in dry THF (400 mL) was cooled to -78° C. and treated with n-butyllithium (133 mL of a 2.5M solution in hexane; 0.3325 mole) over 30 minutes. The mixture was stirred at -78° C. for 30 minutes and treated with 4-fluorobenzophenone (50 g; 0.25 mole). The mixture was stirred at -78° C. for 30 minutes and allowed to warm up to 23° C. over 2 hours. The reaction was quenched with 2N HCl (100 mL) and the organic solvent was removed by evaporation. The residue was extracted with CHCl3 (2×100 mL) and the combined organic layers were dried (Na2SO4) and evaporated to afford a brown oil. Purification by chromatography using 20% EtOAc-hexane as eluent afforded the title compound as a white solid (46.3 g; 62%). m.p.=113°- 114° C. (crystallized from EtOAc-hexane). MS (CI): m/e=299 for (M+H)+.

1. stirringThe mixture was stirred at -78° C. for 30 minutes
2. temperatureto warm up to 23° C. over 2 hours
3. customThe reaction was quenched with 2N HCl (100 mL)
4. customthe organic solvent was removed by evaporation
5. extractionThe residue was extracted with CHCl3 (2×100 mL)
6. dry with materialthe combined organic layers were dried (Na2SO4)
7. customevaporated
8. customto afford a brown oil
9. customPurification by chromatography