反应详情

温度

100 °C

Methyl 2,3-difluorobenzoate (0.816 g, 4.741 mmol) and 2-(piperidin-1-yl)ethanamine (2.7 mL, 18.93 mmol) were dissolved in DMF (15 mL) and heated in a microwave for 30 mins at 100° C. The reaction mixture was transferred to a separatory funnel with EtOAc (75 mL) the organics washed with 10 ml pure water. The layers were separated and the aqueous layer was extracted with EtOAc (2×50 mL). The crude material was purified by silica gel column chromatography eluting with EtOAc/Hexanes to give methyl 2-(2-(piperidin-1-yl)ethylamino)-3-fluorobenzoate (837 mg, 63%). LC/MS: 281.17 (M+1) Rt=1.63 min (10-90% 3/5 min (grad/run) with formic acid).

1. washthe organics washed with 10 ml pure water
2. customThe layers were separated
3. extractionthe aqueous layer was extracted with EtOAc (2×50 mL)
4. customThe crude material was purified by silica gel column chromatography
5. washeluting with EtOAc/Hexanes