反应详情

To 80 ml of dried tetrahydrofuran cooled with ice was gradually added 5.4 g of pulverized anhydrous aluminium chloride. After stirring for 15 minutes, 7.8 g of sodium azide was added and the mixture was further stirred for 15 minutes. After a temperature of the solution was brought to room temperature, 2.5 g of 3-cyano-2-oxo-8-chromenyloxyacetic acid was added and the mixture was gradually heated to carry out the reaction under reflux for 120 hours. After the reaction was completed, the reaction mixture was poured into a mixture of 20 ml of concentrated hydrochloric acid and 300 ml of ice water to form a precipitate, which was filtered and recrystallized to give a desired compound.

1. stirringthe mixture was further stirred for 15 minutes
2. customwas brought to room temperature
3. temperaturethe mixture was gradually heated
4. customthe reaction
5. temperatureunder reflux for 120 hours
6. customto form a precipitate, which
7. filtrationwas filtered
8. customrecrystallized