反应详情

温度

-20 °C

A solution of N3-(3,5-dichlorophenyl)-1H-1,2,4-triazole-3,5-diamine Intermediate 2 (70 mg, 287 μmol) and 5-chloro-2-formylpyridine (60 mg, 424 μmol) in MeOH (3 ml) was stirred at room temperature for one day and then at 45° C. for two days to give a suspension, cooled to −20° C. and was filtered to collect the solid. The solid was re-suspended in MeOH (5 ml), NaBH4 (163 mg, 4.3 mmol) was added in a few portions and the reaction was stirred for 1 hour. The solvent was removed, and the reaction mixture was redissolved in EtOAc (5 ml) and washed with water (2×4 ml), dried over MgSO4 and concentrated. Crystallization from DCM afforded a white solid as desired product (96.6 mg, 90% yield). MS +m/z: 369 (M+H)+

1. customat 45° C. for two days to give a suspension
2. filtrationwas filtered
3. customto collect the solid
4. customThe solvent was removed
5. dissolutionthe reaction mixture was redissolved in EtOAc (5 ml)
6. washwashed with water (2×4 ml)
7. dry with materialdried over MgSO4
8. concentrationconcentrated
9. customCrystallization from DCM