反应详情

温度

80 °C

2-amino-3-hydroxybenzoic acid (1.2 g, 7.8 mmol) was suspended in 20 ml of THF and at 0° C. CDI (1.9 g, 1.5 equiv.) was added. The mixture was warmed at 80° C. for 5 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 520 mg of an orange solid. Yield=37% 1HNMR (DMSO, 200 MHz) δ 7.45 (3H, m), 10.40 (1H, bs), 12.00 (1H, bs)

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