反应详情

温度

150 °C

(±)-(2-Chloro-5-methoxy-phenyl)-[1-(2,4-dichloro-pyrimidin-5-yl)-ethyl]-amine (70 mg; 0.21 mmol) (from Example 12a supra) was combined with phenyl isocyanate (60 μL; 0.55 mmol) (Aldrich) and heated (neat) at 150° C. for 65 minutes. Thin layer chromatography analysis showed some unreacted starting material remained. Additional isocyanate (20 μL; 0.18 mmol) was added and the mixture heated at 150° C. for an additional 30 minutes. Upon cooling, hexanes was added. After stirring, the supernatant was decanted off and the residue dried to give the intermediate (±)-1-(2-chloro-5-methoxy-phenyl)-1-[1-(2-chloropyrimidin-5-yl)-ethyl]-3-phenyl-urea which contained about 20% starting material by HPLC.

1. temperaturethe mixture heated at 150° C. for an additional 30 minutes
2. temperatureUpon cooling
3. customthe supernatant was decanted off
4. customthe residue dried