反应详情

To a stirred solution of 2-(4-cyanophenyl)-N-((2-m-tolyl-6-(trifluoromethyl)pyridin-3-yl)methyl)propanamide (305 mg, 0.72 mmol) in ethanol was cooled to 0° C. and added NiCl2.6H2O (17 mg, 0.072 mmol) and stirred more then 15 min. Sodium borohydride (191 mg, 5.04 mmol) was then added in small portions. The reaction was exothermic and effervescent. The resulting reaction mixture was allowed to warm to room temperature and left to stir for 2 hour. The mixture was filtered using celite pad. The filtrate was concentrated was evaporated. The residue was dissolved in ethylacetate and washed with water and brine, but when it does not separate easily, small amount of 1N HCl and saturated NaHCO3 was used. The organic layer was dried over magnesium sulfate and filtered. The filtrate removed in vacuo. The crude was purified by column chromatography. 2-(4-(Aminomethyl)phenyl)-N-((2-m-tolyl-6-(trifluoromethyl)pyridin-3-yl)methyl)propanamide (167 mg) was obtained as 64% yield.

1. custom15 min
2. customThe resulting reaction mixture
3. waitleft
4. stirringto stir for 2 hour
5. filtrationThe mixture was filtered
6. concentrationThe filtrate was concentrated
7. customwas evaporated
8. dissolutionThe residue was dissolved in ethylacetate
9. washwashed with water and brine, but when it
10. customdoes not separate easily
11. dry with materialThe organic layer was dried over magnesium sulfate
12. filtrationfiltered
13. customThe filtrate removed in vacuo
14. customThe crude was purified by column chromatography