反应详情

To a solution of 313b (1.0 g, 4.0 mmol) in dichloromethane (30 mL) was added a solution of CH3NH2 (1.07 g, 12.0 mmol, 35% in methanol). This reaction mixture was stirred at room temperature for 3 h and diluted with water (30 mL). The organic layer was separated, dried over Na2SO4, and concentrated under reduced pressure. The residual was purified by silica-gel column chromatography eluting with 30:1 dichloromethane/methanol to afford 313c (450 mg, 57%) as a yellow solid. MS-ESI: [M+H]+ 196.9

1. customThe organic layer was separated
2. dry with materialdried over Na2SO4
3. concentrationconcentrated under reduced pressure
4. customThe residual was purified by silica-gel column chromatography
5. washeluting with 30:1 dichloromethane/methanol