反应详情

3-Bromoprop-1-ene (0.433 mL, 5.00 mmol) was added to a stirred solution of ethyl 4-(1,4-diazepan-1-yl)benzoate (1.242 g, 5 mmol) and DIPEA (2.183 mL, 12.50 mmol) in dichloromethane (20 mL). The reaction mixture was stirred under nitrogen at room temperature for 24 h. This was diluted with dichloromethane (20 mL), washed with water (2×25 ml) and saturated sodium chloride solution (20 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% 2.5M ammonia/MeOH in DCM. Pure fractions were evaporated to dryness to afford ethyl 4-(4-allyl-1,4-diazepan-1-yl)benzoate (0.700 g, 48.5%) as a yellow oil.

1. washwashed with water (2×25 ml) and saturated sodium chloride solution (20 ml)
2. dry with materialdried over MgSO4
3. filtrationfiltered
4. customevaporated to dryness
5. customThe crude product was purified by silica column chromatography
6. washeluting with a gradient of 0 to 5% 2.5M ammonia/MeOH in DCM
7. customPure fractions were evaporated to dryness