反应详情

温度

80 °C

A solution of 2-methyl-5-benzofuranamine·HCl (35 mg, 0.24 mmol), ethyl 2-cyano-3,3-bis(methylthio)-2-propenoate (47 mg, 0.23 mmol), and ethanol (0.4 mL) was heated at 70° C. for 12 h. To the mixture was added 3-aminohexahydro-1-(2-oxo-2-phenylethyl)-2H-azepin-2-one (56 mg, 0.23 mmol). The resulting mixture was heated at 80° C. for 2 days, and then concentrated in vacuo. The residue was purified by preparative HPLC (column-YMC-PACK ODSA S5, 30×250 mm); flow rate 25 mL/min; gradient time 55 min) to give the title compound as a pale yellow solid (8 mg, 7%): MS (ESI, pos. ion spectrum) m/z 501; HPLC (method A) tR 4.26 min.

1. concentrationconcentrated in vacuo
2. customThe residue was purified by preparative HPLC (column-YMC-PACK ODSA S5, 30×250 mm)