反应详情

To a tetrahydrofuran solution of 2M dimethylamine, 2.3M hexane solution of hexyllithium was slowly added over a period of at least three (3) hours while maintaining the temperature at between −8° C. and −12° C. This solution was added to the tetrahydrofuran solution of ethyl-4-cyanobenzoate (F) while maintaining the temperature between −8° C. and −12° C. The completion of the reaction was confirmed by HPLC, and the solution temperature was adjusted to between −8° C. and 3° C. The reaction mixture was slowly added to the cold solution of aqueous sodium bicarbonate solution and the desired ethyl-4-(N,N-dimethylcarbamimidoyl)benzoate (G) was extracted with ethyl acetate. The ethyl acetate layer was dried, filtered and evaporated under vacuum to afford ethyl-4-(N,N-dimethylcarbamimidoyl)benzoate (G) as a white solid.

1. temperaturewhile maintaining the temperature at between −8° C. and −12° C
2. temperaturewhile maintaining the temperature between −8° C. and −12° C
3. customwas adjusted to between −8° C. and 3° C
4. extractionthe desired ethyl-4-(N,N-dimethylcarbamimidoyl)benzoate (G) was extracted with ethyl acetate
5. dry with materialThe ethyl acetate layer was dried
6. filtrationfiltered
7. customevaporated under vacuum