反应详情

温度

135 °C

The mixture consisting of 1.07 g of 4-amino-3-chlorobenzonitrile, 30 ml of xylene and 1.7 g of trimethyltin azide was stirred at 135° C. for 8 hours. After cooling, 25 ml of methanol were added, the mixture was stirred at room temperature for 30 minutes and the volatile constituents were removed on a rotary evaporator. On stirring, a solid precipitated out of the mixture obtained in this way, and was filtered off with suction and briefly dried under reduced pressure. This solid was dissolved in 1N sodium hydroxide solution and filtered, and the product was precipitated by acidifying with 2N hydrochloric acid, filtered off with suction and dried under reduced pressure.

1. temperatureAfter cooling
2. stirringthe mixture was stirred at room temperature for 30 minutes
3. customthe volatile constituents were removed on a rotary evaporator
4. stirringOn stirring
5. customa solid precipitated out of the mixture
6. customobtained in this way
7. filtrationwas filtered off with suction
8. custombriefly dried under reduced pressure
9. dissolutionThis solid was dissolved in 1N sodium hydroxide solution
10. filtrationfiltered
11. customthe product was precipitated
12. filtrationfiltered off with suction
13. customdried under reduced pressure