反应详情

To a solution of ethyl 3-{4-amino-6-[methyl(phenyl)amino]-1,3,5-triazin-2-yl}-1,2,4-oxadiazole-5-carboxylate (prepared in an analogous manner to Example 73, 0.2 g, 0.58 mmol) in toluene (10 mL) at 0 C was added trimethylaluminium (2M in toluene, 0.88 mL, 1.7 mmol) over a period of 5 min and the mixture was then stirred at room temperature for 2 h. 6-Methoxypyridin-3-amine (0.21 g, 1.7 mmol) was added and the mixture was heated to 60 C for 15 h. The mixture was cooled to room temperature and quenched with ice water. The mixture was extracted with EtOAc (3×20 mL) and the organic layers were concentrated under vacuum. The residue was slurried in acetonitrile for 30 min and the resultant precipitate was filtered off to afford the title compound (0.100 g, 43%).

1. temperaturethe mixture was heated to 60 C for 15 h
2. temperatureThe mixture was cooled to room temperature
3. customquenched with ice water
4. extractionThe mixture was extracted with EtOAc (3×20 mL)
5. concentrationthe organic layers were concentrated under vacuum
6. waitThe residue was slurried in acetonitrile for 30 min
7. filtrationthe resultant precipitate was filtered off