反应详情

2-Methoxy-5-sulfamoylbenzoic acid (2.3 g) and triethylamine (1.4 ml) are dissolved in anhydrous tetrahydrofuran (20 ml), and therto is added 1-methanesulfonyloxy-1,2,3-benzotriazole (2.2 g). After stirring at room temperature for 20 minutes, to the mixture is added 1-ethyl-2-aminomethylpyrrolidine (1.3 g) to precipitate oily products with exotherm. The mixture is stirred for 1 hour and then the solvent is distilled off. The resulting oily residue is dissolved in 1 N hydrochloric acid and the solution is washed twice with ethyl acetate. The aqueous layer is distilled under a reduced pressure to remove the remaining ethyl acetate and made alkaline with aqueous ammonia. The resulting precipitates are separated by filtration, washed with diluted aqueous ammonia and dried to give 1-ethyl-2-(2-methoxy-5-sulfamoylbenzamidomethyl)pyrrolidine (2.2 g), melting point: 175°-177° C.

1. customto precipitate oily products with exotherm
2. stirringThe mixture is stirred for 1 hour
3. distillationthe solvent is distilled off
4. dissolutionThe resulting oily residue is dissolved in 1 N hydrochloric acid
5. washthe solution is washed twice with ethyl acetate
6. distillationThe aqueous layer is distilled under a reduced pressure
7. customto remove the remaining ethyl acetate
8. customThe resulting precipitates
9. customare separated by filtration
10. washwashed with diluted aqueous ammonia
11. customdried