反应 #3662340
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06215002B1
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of ethyl bromocrotonate (193 mg), piperidine (94 mg) and potassium carbonate (276 mg) in acetonitrile (10 ml) was stirred and heated at reflux for 3 hours. The reaction mixture was cooled and the solvent was removed in vacuo. The residue was partitioned between water (2×15 ml) and ethyl acetate (20 ml). The organic extracts were dried (Na2SO4), filtered and concentrated in vacuo to give the title compound as an orange oil (157 mg). Tlc Silica. (100:8:1)Mixture of dichloromethane, ethanol and ammonia (S.G=0.88) Rf=0.55 Mass spec MH+ (found)=198 MH+ (calculated)=198. heated at reflux for 3 hours The reaction mixture was cooled the solvent was removed in vacuo The residue was partitioned between water (2×15 ml) and ethyl acetate (20 ml) The organic extracts were dried (Na2SO4) filtered concentrated in vacuo
来源 ID: ord-8c97c5b68c9a465d84f567e6d5e446cc