反应详情

To a solution of 5-benzhydrylthio-1H-tetrazole (29 g) in tetrahydrofuran (145 ml) were added triethylamine (12.0 g) and 2-propynyl bromide (19.3 g) at room temperature. The resulting mixture was stirred for 2.5 hours at 40° to 45° C. The reaction mixture was filtered and the filtrate was evaporated. The residue was shaken with a mixture of ethyl acetate and water. The ethyl acetate layer was separated, washed with a saturated aqueous solution of sodium chloride, dried over magnesium sulfate and then evaporated. The residual oil (27.7 g) was subjected to column chromatography on silica gel, and eluted with a mixture of n-hexane, chloroform and ethyl acetate (5.5:4.5:0.5), to give 5-benzhydrylthio-2-(2-propynyl)-2H-tetrazole (14.2 g), mp 85° to 86° C.

1. filtrationThe reaction mixture was filtered
2. customthe filtrate was evaporated
3. stirringThe residue was shaken with a mixture of ethyl acetate and water
4. customThe ethyl acetate layer was separated
5. washwashed with a saturated aqueous solution of sodium chloride
6. dry with materialdried over magnesium sulfate
7. customevaporated
8. washeluted with a mixture of n-hexane, chloroform and ethyl acetate (5.5:4.5:0.5)