反应 #1687465
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08618132B2
反应条件: temp:75.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 0.51 mL (4.23 mmol) 1,4-dibromobutane in 20 mL acetonitrile is added slowly to a solution of 1.0 g (4.23 mmol) 4-bromo-phenethylamine hydrochloride, 1.8 g (13.0 mmol) K2CO3 and 200 mg (1.20 mmol) Kl in 100 mL acetonitrile at 75° C. and the reaction mixture is stirred for a further 4 h at 75° C. The reaction solution is diluted with 100 mL water and the aqueous phase is extracted with 100 mL EtOAc. The combined organic extracts are washed with saturated NaCl solution, the organic phase is dried over Na2SO4 and the solvent is eliminated i.vac. Further purification is carried out by column chromatography on silica gel (EtOAc/MeOH/NH3 9:1:0.1) the aqueous phase is extracted with 100 mL EtOAc The combined organic extracts are washed with saturated NaCl solution the organic phase is dried over Na2SO4 Further purification
来源 ID: ord-488fc83eb3934255bdcf9f36d0e594e6