反应详情

温度

90 °C

DMF (0.06 ml, cat) was added to a solution of 4-chloro-2-nitro-benzenesulfonic acid (600 mg, 2.5 mmol) in SOCl2 (3.1 ml) and the mixture was heated at 90° C. for 3 h. After cooling, the solvent was removed in vacuo. The mixture was diluted with water and extracted repeatedly with chloroform. The combined organic layers were washed with saturated NaHCO3 solution, dried (Na2SO4) and concentrated in vacuo to give the title compound (560 mg) which was used in the next step without further purification. The structure was confirmed by 1H NMR.

1. temperatureAfter cooling
2. customthe solvent was removed in vacuo
3. additionThe mixture was diluted with water
4. extractionextracted repeatedly with chloroform
5. washThe combined organic layers were washed with saturated NaHCO3 solution
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated in vacuo