反应详情

In a mixture of 20 ml of dichloromethane and 3.4 g (33.6 mmol) of triethylamine was dissolved 1.50 g (10.6 mmol) of ethyl tetrazol-5-carboxylate, and 3.75 g (34.6 mmol) of ethyl chloroformate was added dropwise at 0° C. After stirring overnight at 0° C. to room temperature, water was added to the reaction mixture, followed by phase separation. Then, the dichloromethane layer was successively washed with 5% sodium dihydrogenphosphate solution, 5% sodium hydrogencarbonate solution and water, dried with magnesium sulfate, and concentrated, which afforded 1.42 g of ethyl N-ethoxycarbonyltetrazol-5-carboxylate. Yield, 63%.

1. additionwas added dropwise at 0° C
2. customfollowed by phase separation
3. washThen, the dichloromethane layer was successively washed with 5% sodium dihydrogenphosphate solution, 5% sodium hydrogencarbonate solution and water
4. dry with materialdried with magnesium sulfate
5. concentrationconcentrated