反应详情

A mixture of 130 g. (1 mole) of ethyl azidoacetate prepared as described in part A and 96 g. (1.56 mole) of cyanogen chloride was heated at a temperature of 125° C. for 20 hours. After the reaction mixture had cooled, the reaction product mixture was dissolved in ethyl acetate, and the solution was filtered and evaporated in vacuo yielding a yellow crystalline mass of product. The yellow crystals were recrystallized from aqueous ethyl alcohol and gave 149 g. (78% yield) of ethyl 5-chloro-1H-tetrazol-1-ylacetate as pale yellow crystals melting at about 57°-60° C.

1. additionA mixture of 130 g
2. temperatureAfter the reaction mixture had cooled
3. filtrationthe solution was filtered
4. customevaporated in vacuo
5. customyielding a yellow crystalline mass of product
6. customThe yellow crystals were recrystallized from aqueous ethyl alcohol
7. customgave 149 g