反应详情

To a solution of 5-phenyl-1H-tetrazole (500 mg, 3.42 mmol) in 10 mL of dry tetrahydrofuran was added dropwise s-butyllithium (1.04 mol/L, 6.6 mL, 6.9 mmol) under nitrogen at −78° C. After the reaction mixture was stirred at the same temperature for 30 min, N,N-dimethylformamide (2 mL, 30 mmol) was added dropwise. After the reaction mixture was stirred at room temperature for 10 min, 1M HCl (10 mL) was added. The solution was allowed to warm up to room temperature, diluted with ethyl acetate, and extracted. The extract was washed with brine, and dried over MgSO4. After filtration, the filtrate was concentrated in vacuo, and the residue was purified by recrystallization (hexane 2.5 mL, ethyl acetate 2.5 mL) to obtain the title compound (390 mg, 99%).

1. stirringAfter the reaction mixture was stirred at room temperature for 10 min
2. extractionextracted
3. washThe extract was washed with brine
4. dry with materialdried over MgSO4
5. filtrationAfter filtration
6. concentrationthe filtrate was concentrated in vacuo
7. customthe residue was purified by recrystallization (hexane 2.5 mL, ethyl acetate 2.5 mL)