反应详情

温度

90 °C

5-(1-(t-Butoxycarbonyl)-1,2,3,6-tetrahydropyrid-4-yl)-7-(2-chloro-4-pyridyl)-8-(3-(trifluoromethyl)phenyl)-1,2,4-triazolo[4,3-c]pyrimidine (0.93 g, 1.7 mmol), (S)-α-methylbenzylamine (0.48 g, 4 mmol), palladium acetate (0.06 g, 0.26 mmol) and racemic BINAP (0.16 g, 0.26 mmol) were combined in toluene (15 ml) and the resulting solution was degassed with nitrogen. Sodium t-butoxide (0.48 g, 5 mmol) was added and the resulting mixture was heated to 90° C. for 1 hour. The mixture was partitioned between sat. ammonium chloride and ethyl acetate. The organic layer was separated, dried over sodium sulfate, filtered and concentrated to a syrup. The residue was purified by column chromatography on silica gel (30% ethyl acetate in hexane) gave the product as a syrup; MS m/z (M+H)+ 642.4; C35H34F3N7O2 require 641.3.

1. customthe resulting solution was degassed with nitrogen
2. customThe mixture was partitioned between sat. ammonium chloride and ethyl acetate
3. customThe organic layer was separated
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated to a syrup
7. customThe residue was purified by column chromatography on silica gel (30% ethyl acetate in hexane)