反应详情

A solution of cyanogen bromide (3.2 g, 0.030 mol) in 100 ml. 2-methoxyethanol was added to a solution of N-(6-amino-2,3-dichlorobenzyl)glycine ethyl ester (8.2 g, 0.030 mol) in 250 ml. 2-methoxyethanol. The solution was stirred at room temperature for 1 hour, heated at reflux for 22 hours, and cooled. The precipitate was filtered off, washed with ether and air dried to give 3.11 gms. of the crude title product (31% yield as the hydrobromide salt). Recrystallization from ethanolic HCl gave the pure title product in 71% recovery (22% overall yield); m.p. >250°.

1. temperatureheated
2. temperatureat reflux for 22 hours
3. temperaturecooled
4. filtrationThe precipitate was filtered off
5. washwashed with ether and air
6. customdried
7. customto give 3.11 gms
8. customRecrystallization from ethanolic HCl