反应详情

Add 2-chloro-N-(3-fluoro-4-nitro-phenyl)-N-methyl-pyridin-4-amine (190 mg, 0.68 mmol), cyclopropanecarboxamide (85 mg, 2.03 mmol), Cs2CO3 (440 mg, 1.35 mmol), (±)-2,2′-bis(diphenylphosphino)-1,1′-binaphthalene (BINAP, 43 mg, 0.05 mmol) and tris(dibenzylideneacetone)dipalladium [Pd2(dba)3, 42 mg, 0.07 mmol] in 1,4-dioxane (6 mL) under N2. Heat the reaction at 125° C. for 16 hrs. TLC (EtOAc:PE=2:1) shows the reaction is complete. Cool to room temperature, filter, and concentrate the filtrate under reduced pressure to give the crude product. Purification by chromatography (silica gel, EtOAc:PE=2:1) affords the target compound (160 mg, 71.7%). MS: (M+1): 331.

1. temperatureHeat
2. customthe reaction at 125° C. for 16 hrs
3. filtrationfilter
4. concentrationconcentrate the filtrate under reduced pressure
5. customto give the crude product
6. customPurification by chromatography (silica gel, EtOAc:PE=2:1)