反应详情

A solution of N3-(3,5-dichlorophenyl)-1H-1,2,4-triazole-3,5-diamine Intermediate 2 (70 mg, 287 μmol) and furfural (85.1 mg, 886 μmol) in MeOH (3 ml) was stirred at room temperature for 3 days. The resulting suspension was filtered to collect the solid. The solid was re-suspended in MeOH (5 ml), NaBH4 (65.1 mg, 1.72 mmol) was added and the reaction was stirred for 1 hour. The solvent was removed, and the reaction mixture was redissolved in DCM and washed with water (2×4 ml), dried over MgSO4 and concentrated to give a solid. Trituration with DCM/Hexanes afforded a white solid as desired product (50.5 mg, 54% yield). MS +m/z: 324 (M+H)+

1. filtrationThe resulting suspension was filtered
2. customto collect the solid
3. customThe solvent was removed
4. dissolutionthe reaction mixture was redissolved in DCM
5. washwashed with water (2×4 ml)
6. dry with materialdried over MgSO4
7. concentrationconcentrated
8. customto give a solid