反应详情

2-amino-3-hydroxybenzoic acid (1 g, 6.5 mmol) was dissolved in 20 ml of DMF and at 0° C. EDCI (1.4 g, 1.2 equiv.), hydroxybenzotriazole (1 g, 1.2 equiv.) and amine 2c (2 g, 1.2 equiv.) were added. The mixture was stirred at rt for 20 hours. The solvent was evaporated and the crude was dissolved in AcOEt (30 ml) and washed with water (1×20 ml) and brine. The organic phase was dried over sodium sulfate and concentrated under vacuum. The purification of the crude residue by crystallization from EtOAc/ether gave 1.6 g of a beige solid. Yield=62.5% [M+1] 393.4 (C20H22F3N3O2 requires 393.4).

1. customThe solvent was evaporated
2. dissolutionthe crude was dissolved in AcOEt (30 ml)
3. washwashed with water (1×20 ml) and brine
4. dry with materialThe organic phase was dried over sodium sulfate
5. concentrationconcentrated under vacuum
6. customThe purification of the crude residue
7. customby crystallization from EtOAc/ether