反应详情

4-Bromo-2-fluorobenzoic acid (5.00 g, 22.8 mmol, 1.00 equiv) and EDC (5.23 g, 27.4 mmol, 1.20 equiv) were dissolved in dichloromethane (100 mL). Morpholine (4.77 mL, 54.8 mmol, 2.40 equiv) was added and the solution was maintained at room temperature for 19 h. The reaction mixture was concentrated en vacuo and diluted with EtOAc and 1N HCl. The phases were separated and the organic phase was washed sequentially with water, saturated NaHCO3, and saturated NaCl. The organic phase was subsequently dried over Na2SO4, filtered and concentrated to afford 5.06 g (81%) of a colorless oil which was used without further purification in the next step. MS (ES) m/e 289 [M+H]+.

1. concentrationThe reaction mixture was concentrated en vacuo
2. additiondiluted with EtOAc and 1N HCl
3. customThe phases were separated
4. washthe organic phase was washed sequentially with water, saturated NaHCO3, and saturated NaCl
5. dry with materialThe organic phase was subsequently dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated