反应详情

温度

170 °C

Trifluoromethanesulfonic acid 1-ethyl-3,3,5-trimethyl-2,4-dioxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepine-7-yl ester(0.12 g), zinc cyanide(70 mg), tris(dibenzylideneacetone) dipalladium 7 mg), 1,1′-bis(diphenylphosphino) ferrocene(8 mg), and zinc powder(2 mg) were added to DMF (1 ml), and the mixture was heated for 20 minutes at 170° C. (microwave reactor). The reaction liquid was cooled to room temperature, and subjected to celite filtration. The filtrate was condensed under reduced pressure, and the residue was purified by silica gel column chromatography (hexane: ethyl acetate=50:50→0:100). The purified product was condensed under reduced pressure to give the title compound(77 mg) as a white solid.

1. customThe reaction liquid
2. temperaturewas cooled to room temperature
3. filtrationsubjected to celite filtration
4. customcondensed under reduced pressure
5. customthe residue was purified by silica gel column chromatography (hexane: ethyl acetate=50:50→0:100)
6. customcondensed under reduced pressure