反应详情

The mixture of ethyl 3-aminobenzoate (3.0 g), tri(ethoxy)methane (3.0 ml) and sodium azide (1.2 g) in acetic acid (30 ml) was stirred for 5 hours at 60°-70° C. To the reaction mixture was added water and the mixture was adjusted to pH 8 with potassium carbonate. The isolated precipitate was collected by filtration and the precipitate was dissolved in a mixture of ethyl acetate and tetrahydrofuran. The mixture was washed with water, dried over magnesium sulfate and evaporated in vacuo. The residue was recrystallized from a mixture of ethanol and diisopropyl ether to give ethyl 3-(1H-tetrazol-1-yl)benzoate (2.44 g).

1. filtrationThe isolated precipitate was collected by filtration
2. dissolutionthe precipitate was dissolved in a mixture of ethyl acetate and tetrahydrofuran
3. washThe mixture was washed with water
4. dry with materialdried over magnesium sulfate
5. customevaporated in vacuo
6. customThe residue was recrystallized from a mixture of ethanol and diisopropyl ether