反应详情

温度

60 °C

To a solution of CH3NH2 in EtOH (0.25 mL) was added TEA (0.5 mL) and 8-(bromomethyl)-N-(2-chlorophenyl)-N-methyl-4,5-dihydrobenzo[b]thieno[2,3-d]oxepine-2-carboxamide (250 mg). The reaction mixture was stirred for 2 h at 60° C. before added water. The mixture was extracted with EtOAc (20 mL×3), dried over Na2SO4 and filtered. The filtrate was concentrated to give the crude product, which was purified by preparative TLC (CH2Cl2: MeOH=10:1) to afford 243 as a light yellow solid (95.6 mg, 42.8%). MS: (ESI+) 412.9

1. extractionThe mixture was extracted with EtOAc (20 mL×3)
2. dry with materialdried over Na2SO4
3. filtrationfiltered
4. concentrationThe filtrate was concentrated
5. customto give the crude product, which
6. customwas purified by preparative TLC (CH2Cl2: MeOH=10:1)