反应详情

温度

100 °C

Ethyl 4-fluorobenzoate (11.01 mL, 75 mmol) and 1,4-diazepane (30.0 g, 300.00 mmol) in DMSO (150 mL) warmed to 100° C. under nitrogen. The resulting solution was stirred at 100° C. for 24 h. The reaction mixture was cooled and evaporated to dryness. The reaction mixture was quenched with 2M NaOH (150 mL), extracted with EtOAc (3×75 mL), the organic layer was washed with saturated brine (100 ml), dried over MgSO4, filtered and evaporated to afford ethyl 4-(1,4-diazepan-1-yl)benzoate (17.43 g, 94%) as a colourless oil.

1. temperatureThe reaction mixture was cooled
2. customevaporated to dryness
3. customThe reaction mixture was quenched with 2M NaOH (150 mL)
4. extractionextracted with EtOAc (3×75 mL)
5. washthe organic layer was washed with saturated brine (100 ml)
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. customevaporated