反应详情

A solution of ethyl 4-fluorobenzoate (0.293 mL, 2 mmol) and 1-isopropyl-1,4-diazepane (0.539 mL, 4.00 mmol) in dimethylsulfoxide (10 mL), was heated at 120° C. for 18 h. The reaction mixture was diluted with water (75 ml) and extracted with ethyl acetate (3×25 ml). The extracts were washed with saturated sodium chloride solution (50 ml), dried over MgSO4, filtered and evaporated to dryness. The crude product was purified by silica column chromatography, eluting with a gradient of 0 to 5% MeOH in DCM. Pure fractions were evaporated to dryness to afford ethyl 4-(4-isopropyl-1,4-diazepan-1-yl)benzoate (0.212 g, 36.5%) as a yellow oil.

1. extractionextracted with ethyl acetate (3×25 ml)
2. washThe extracts were washed with saturated sodium chloride solution (50 ml)
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. customevaporated to dryness
6. customThe crude product was purified by silica column chromatography
7. washeluting with a gradient of 0 to 5% MeOH in DCM
8. customPure fractions were evaporated to dryness