反应详情

Triphosgene (0.042 g, 0.140 mmol) was added to a solution of 1-(4-Chloro-phenyl)-5-trifluoromethyl-1H-pyrazol-4-ylamine (0.100 g, 0.382 mmol) and Na2CO3 (0.405 g, 3.82 mmol) in CH2Cl2/H2O (50 mL, 1:1) and stirred at room temperature for 30 min. 3-Methanesulfonyl-phenylamine HCl (0.095 g, 0.458 mmol) was added to the reaction mixture, stirred at room temperature for 2 hrs, organic layer collected and aqueous layer extracted with EtOAc (3×25 mL). Organic layers were collected, concentrated and crude product purified by column chromatography to give 1-[1-(4-chloro-phenyl)-5-trifluoromethyl-1H-pyrazol-4-yl]-3-(3-methanesulfonyl-phenyl)-urea (0.040 g, 22%).

1. stirringstirred at room temperature for 2 hrs
2. customorganic layer collected
3. extractionaqueous layer extracted with EtOAc (3×25 mL)
4. customOrganic layers were collected
5. concentrationconcentrated
6. customcrude product purified by column chromatography