反应 #2934129
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09102688B2
反应条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 1,3-dimethyl-5,5-dimethylhydantoin (0.73 g, 36.7 mmol) was added to a solution of 9-fluoro-5H-6-thia-4,5-diaza-chrysene 6,6-dioxide 187 (1.0 g, 33.3 mmol) in chloroform (40 ml) and the reaction was heated at 70° C. until the starting material was consumed (LCMS). After cooling, the mixture was concentrated in vacuo. The residue was dissolved in EtOAc and the organic phase was washed with sodium metabisulfate, water and brine. The organic phase was dried (Na2SO4) and concentrated in vacuo. The crude residue was purified by column chromatography with DCM/MeOH (99:1) as the eluent to give the title compound (0.8 g, 69%). was consumed (LCMS) After cooling the mixture was concentrated in vacuo The residue was dissolved in EtOAc the organic phase was washed with sodium metabisulfate, water and brine The organic phase was dried (Na2SO4) concentrated in vacuo The crude residue was purified by column chromatography with DCM/MeOH (99:1) as the eluent
来源 ID: ord-8bc46504056948c28e1870549b252ddf