反应详情

107.5 mg (0.34 mmol) of the free base of 2-[2,2-difluoro-2-(3-butoxyphenyl)-ethylamino]-N,N-dimethyl-acetamide (see Example 1-1) are dissolved in dry THF (10 mL). To this solution, formaldehyde (36.5% water solution, 52.1 μL; 0.69 mmol), acetic acid (2.5 mL), and MP-CNBH3 (2.3 mmol/g; 325 mg; 0.75 mmol) are added sequentially. After stirring 1 hour the reaction is completed. After further stirring for 1.5 hours, the reaction mixture is evaporated. The crude residue is flash-chromatographed on silica gel using DCM/MeOH (99.5/0.5) as an eluant. 73.1 mg (65%) of pale yellow fluid 2-{[2,2-difluoro-2-(3-butoxyphenyl)-ethyl]-methylamino}-N,N-dimethyl-acetamide are obtained.

1. stirringAfter further stirring for 1.5 hours
2. customthe reaction mixture is evaporated
3. customThe crude residue is flash-chromatographed on silica gel