反应详情

温度

50 °C

To a solution of 150 mg (0.25 mmol) of the above 5-chloro-7-[2-(3-chloro-pyridin-2-yl)-5-trifluoromethyl-2H-pyrazol-3-yl]-3-methyl-1H-8-oxa-1,2,6-triaza-cyclopenta[a]naphthalen-9-one in 3 mL of N,N-dimethylformamide is added 100 mg (0.75 mmol) of bicyclopropyl-1-ylamine hydrochloride and 104 μL (0.75 mmol) of triethylamine. The reaction is stirred at 50° C. for 24 hours and then concentrated in vacuo. The residue is taken-up with acetone and after filtration the filtrate is evaporated. Purification of the residue by flash chromatography (SiO2, hexanes/ethyl acetate 3:2) affords 70 mg (48%) of a solid; LC/MS:578/580 (M+H)+, m.p.: 228-229° C.

1. concentrationconcentrated in vacuo
2. filtrationafter filtration the filtrate
3. customis evaporated
4. customPurification of the residue by flash chromatography (SiO2, hexanes/ethyl acetate 3:2)