反应详情

A DCE solution (33 mL) of 2-bromo-6-chloro-4-(trifluoromethyl)benzaldehyde (3.7 g, 12.9 mmol), 2′,4′-dichloro-[1,1′-biphenyl]-4-amine (3.4 g, 14.4 mmol), and HOAc (3.0 mL) was heated to 70° C. After 10 min the homogeneous solution was cooled to room temperature and solid NaBH(OAc)3 (5.46 g, 25.8 mmol) was added and the resulting mixture was warmed to 40° C. After 30 min, EtOAc and 2 M K2CO3 were added and the layers were separated. The aqueous layer was extracted with EtOAc. The combined organic layers were washed with 4 M NaCl, dried (Na2SO4), concentrated, and purified via column chromatography to yield the title compound.

1. temperaturethe resulting mixture was warmed to 40° C
2. customthe layers were separated
3. extractionThe aqueous layer was extracted with EtOAc
4. washThe combined organic layers were washed with 4 M NaCl
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated
7. custompurified via column chromatography