反应详情

温度

90 °C

95 mg (0.27 mmol) of 2,4-dichloro-5-(2-chloro-4,6-difluorophenylamino)benzoic acid were boiled with 0.98 ml of thionyl chloride under reflux for 3 hours. The thionyl chloride was distilled off, and the residue was mixed with 3 ml of toluene and concentrated in vacuo. The residue was taken up in 2 ml of toluene and added to a solution of 39 mg (0.27 mmol) of ethyl 3-dimethylaminoacrylate, 6 μl of triethylamine and 1 ml of toluene. The mixture was heated at 90° C. for 3 hours. The mixture was concentrated and chromatographed on silica gel (heptane:ethyl acetate=75:25 to 0:100 in 45 minutes). 30 mg (23%) of the desired product were obtained.

1. temperatureunder reflux for 3 hours
2. distillationThe thionyl chloride was distilled off
3. additionthe residue was mixed with 3 ml of toluene
4. concentrationconcentrated in vacuo
5. concentrationThe mixture was concentrated
6. customchromatographed on silica gel (heptane:ethyl acetate=75:25 to 0:100 in 45 minutes)