反应详情

温度

0 °C

2-Amino-4,5-dichloro-benzoic acid (1.5 g, 7.28 mmol) was dissolved in 1:1 DCM/THF (20 mL) and cooled to 0° C. Phosgene (20% in toluene, 5.4 mL, 8.00 mmol) and Hünig's base (2.54 mL, 14.6 mmol) were added and the reaction was stirred overnight and warmed slowly to rt. The mixture was poured into water and extracted with DCM (3×) and EtOAc (2×). The combined organic layers were dried (MgSO4), and concentrated to provide the product as a white solid (1.6 g, 92%). HPLC: RT=8.10 min. MS (ESI−): mass calcd. for C8H3Cl2NO3, 232.0; m/z found, 231 [M−H]−. 1H NMR (400 MHz, DMSO-d6): 11.95 (s, 1H), 8.10 (s, 1H), 7.32 (s, 1H).

1. temperaturewarmed slowly to rt
2. extractionextracted with DCM (3×) and EtOAc (2×)
3. dry with materialThe combined organic layers were dried (MgSO4)
4. concentrationconcentrated