反应 #3577747
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05652247
反应条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a mixture of N-(1-benzyl-4-piperidinyl)aniline (1.8 g), diisopropyl ether (20 ml) and triethylamine (0.87 g) is added dropwise a solution of β-n-butoxyacrylic acid chloride (1.4 g) in diisopropyl ether (5 ml) with stirring and heating at 70° C. After completion of dropwise addition, the mixture is further stirred with heating at the same temperature for 0.5 hour. After cooling, water is added to the reaction mixture and the mixture is subjected to extraction with ethyl acetate. The extract is washed with water and dried over magnesium sulfate. The solvent is distilled off under reduced pressure and the resulting residue is purified by silica gel column chromatography give N-(β-n-butoxyacryloyl)-N-(1-benzyl-4-piperidinyl)aniline (2.6 g). After completion of dropwise addition the mixture is further stirred with heating at the same temperature for 0.5 hour After cooling the mixture is subjected to extraction with ethyl acetate The extract is washed with water dried over magnesium sulfate The solvent is distilled off under reduced pressure the resulting residue is purified by silica gel column chromatography
来源 ID: ord-76524ef1d09d412fbfaee85ea7211d6a