反应详情

温度

60 °C

A mixture of 1-phenyl-5-mercapto-1H-tetrazole (3.5 g, 19.64 mmol), (2-methyl-2-oxiranylmethyl) toluene-4-sulfonate (5 g, 20.64 mmol), potassium carbonate (3 g, 21.71 mmol), and sodium iodide (4.5 g, 30.02 mmol) in DMF (30 ml) was stirred at 60° C. for 6 hours. The reaction mixture was was poured into water, and extracted with ethyl acetate twice. The extracts were combined, washed with 5% sodium hydroxide aqueous solution and then with water three times, and dried over sodium sulfate. After filtration, the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (n-hexane/ethyl acetate=2/1) to afford 5-(2-methyl-2-oxiranylmethylsulfanyl)-1-phenyl-1H-tetrazole (1.9 g, yield 39%) as a colorless oil.

1. extractionextracted with ethyl acetate twice
2. washwashed with 5% sodium hydroxide aqueous solution
3. dry with materialwith water three times, and dried over sodium sulfate
4. filtrationAfter filtration
5. concentrationthe filtrate was concentrated under reduced pressure
6. customThe residue was purified by silica gel column chromatography (n-hexane/ethyl acetate=2/1)