反应 #2939798
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09115132B2
反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 1H-1,2,3-benzotriazole-1-carbaldehyde (327 mg, 2.22 mmol, Sigma-Aldrich) was added to a solution of 2,4-dichloroaniline (300 mg, 1.85 mmol) in tetrahydrofuran (THF) (6 mL). The solution was heated to 60° C. and stirred for 22.5 h before concentrating in vacuo. The resulting solid was dissolved in DCM (30 ml), washed with 2M HCl (15 ml), the organic layer was passed through a hydrophobic frit and reduced in vacuo. Purification was carried out by silica column chromatography (Biotage SP4, gradient elution 0-100% EtOAc in iso-hexane) to yield the title compound (334 mg). before concentrating in vacuo The resulting solid was dissolved in DCM (30 ml) washed with 2M HCl (15 ml) Purification was carried out by silica column chromatography (Biotage SP4, gradient elution 0-100% EtOAc in iso-hexane)
来源 ID: ord-03817dbdcfdd4fddb916629078477a24