盐酸阿那格雷

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 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°. heated at reflux for 22 hours cooled The precipitate was filtered off washed with ether and air dried to give 3.11 gms Recrystallization from ethanolic HCl

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 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°. heated at reflux for 22 hours cooled The precipitate was filtered off washed with ether and air dried to give 3.11 gms Recrystallization from ethanolic HCl