反应详情

温度

80 °C

A mixture of 38.1 parts of 4-oxo-7-(3-[2-propylphenoxy]-propoxy)-4H-1-benzopyran-2-carbonitrile, 7.52 parts of sodium azide, 6.16 parts of ammonium chloride and 5,000 parts of dimethylformamide was stirred at 80° C for 15 hours. The reaction mixture was cooled and 2,000 parts of 2N hydrochloric acid were added to give a yellow solid which was collected. This product was dissolved in hot 3% sodium bicarbonate solution and the hot solution filtered and then cooled. The solid obtained was collected, washed with water and slurried with 500 parts of 2N hydrochloric acid. The resulting solid was collected, washed with water, dried and crystallised from acetone to give 18.4 parts of 5-(4-oxo-7-[3-{2-propylphenoxy}-propoxy]-4H-1-benzopyran-2-yl)-tetrazole m.pt. 191°-193°.

1. temperatureThe reaction mixture was cooled
2. customto give a yellow solid which
3. customwas collected
4. dissolutionThis product was dissolved in hot 3% sodium bicarbonate solution
5. filtrationthe hot solution filtered
6. temperaturecooled
7. customThe solid obtained
8. customwas collected
9. washwashed with water
10. customThe resulting solid was collected
11. washwashed with water
12. customdried
13. customcrystallised from acetone