甲基 2-(氨基甲基)丁酸乙酯

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Methyl 1-cyano-4-hydroxy-7-phenoxyisoquinoline-3-carboxylate (60 mg, 0.19 mmol) and 2-aminomethyl-butyric acid methyl ester (crude, 1.57 mmol) in MeOH (3 mL) were heated at 150° C. in a microwave for 3 hours. The solvent was removed in vacuo and the residue oil was purified by flash chromatography (0-50% EtOAc/hexanes) to give the title compound in 55 mg. MS: (−) m/z 418.14 (M−1). The solvent was removed in vacuo the residue oil was purified by flash chromatography (0-50% EtOAc/hexanes)

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a slurry of Raney-Ni (1.9 g, 50% in H2O, rinsed 3 times with EtOH before use) in EtOH (20 mL) was added methyl 2-cyanobutanoate (200 mg, 1.57 mmol). The resulting mixture was stirred under a hydrogen atmosphere at room temperature for 20 hours. The liquid was then carefully decanted into another flask and the metal was washed twice with EtOH. The combined EtOH solution was concentrated in vacuo to give the title compound in 200 mg, which was used in the subsequent step without further purification. The liquid was then carefully decanted into another flask the metal was washed twice with EtOH The combined EtOH solution was concentrated in vacuo