反应详情

温度

80 °C

In a sealed tube a mixture of 2-bromo-3-chloro-4,5-difluorobenzoic acid (Example 20, 7.96 g, 29.3 mmol), cyclopropyl amine (4.20 mL, 58.7 mmol), potassium acetate (5.77 g, 58.6 mmol), cupric acetate monohydrate (0.50 g, 2.5 mmol), and triethylamine (4.9 mL, 35.19 mmol) in isopropyl alcohol is stirred at 80° C. After 16 hours, the reaction mixture is concentrated under vacuum, and the resulting residue is dissolved in ethyl acetate. The organic layer is washed with 1.0 M hydrochloric acid, water, and brine. The organic layer is dried over MgSO4 and filtered. The filtrate is concentrated under vacuum and purified via flash column chromatography (5% isopropyl alcohol/1% formic acid/94% dichloromethane) to afford the title compound (4.62 g). MS CI: m/z 248 (MH+).

1. concentrationthe reaction mixture is concentrated under vacuum
2. dissolutionthe resulting residue is dissolved in ethyl acetate
3. washThe organic layer is washed with 1.0 M hydrochloric acid, water, and brine
4. dry with materialThe organic layer is dried over MgSO4
5. filtrationfiltered
6. concentrationThe filtrate is concentrated under vacuum
7. custompurified via flash column chromatography (5% isopropyl alcohol/1% formic acid/94% dichloromethane)