反应详情

温度

45 °C

To a solution of 4-[3-(5-tert-butyl-2-methyl-2H-pyrazol-3-yl)-ureido]benzoic acid (0.08 g, 0.26 mmol) in a mixture of dichloromethane (4 mL) and DMF (0.20 mL) is added 1-(4-pyridinylmethyl)piperazine (0.046 g, 0.26 mmol), PS-DCC (0.41 g, 0.52 mmol) and HOBT (0.035 g, 0.26 mmol). The mixture is stirred overnight at 45° C. in a closed tube (orbital stirring). Then PS-Trisamine is added (0.52 mmol) and the mixture is stirred for 4 hr at room temperature, filtrated, and washed three times with dichloromethane. The solvents are evaporated under reduced pressure and the residue is purified by biotage column chromatography (eluent: ethyl acetate/methanol 10:1) to give 0.020 g (0.04 mmol), 16% as white solid. ES+(m/z)=476 [M+H].

1. stirring(orbital stirring)
2. stirringthe mixture is stirred for 4 hr at room temperature
3. filtrationfiltrated
4. washwashed three times with dichloromethane
5. customThe solvents are evaporated under reduced pressure
6. customthe residue is purified by biotage column chromatography (eluent: ethyl acetate/methanol 10:1)
7. customto give 0.020 g (0.04 mmol), 16% as white solid