反应详情

温度

150 °C

A mixture of 4-bromo-2-((1-carboxyethyl)amino)-5-fluorobenzoic acid (D86) (1.599 g, 5.22 mmol), sodium acetate (1.714 g, 20.90 mmol) and acetic anhydride (19.72 mL, 209 mmol) was heated at 150° C. for 30 min in a microwave. The mixture was evaporated in vacuo. The residue was diluted with DCM and poured into saturated NaHCO3 aq. (200 mL). The mixture extracted with DCM (30 mL×3). The organic layers were combined, washed with brine (100 mL), filtered through phase separator and evaporated in vacuo. The crude residue was purified by chromatography on silica, eluting with a gradient of 0-35% ethyl acetate in cyclohexane to give title compound (1.233 g). LCMS (A): m/z (M+H)+ 328/330, C13H11BrFNO3 requires 327/329 (acidic).

1. customThe mixture was evaporated in vacuo
2. additionThe residue was diluted with DCM
3. additionpoured into saturated NaHCO3 aq. (200 mL)
4. extractionThe mixture extracted with DCM (30 mL×3)
5. washwashed with brine (100 mL)
6. filtrationfiltered through phase separator
7. customevaporated in vacuo
8. customThe crude residue was purified by chromatography on silica
9. washeluting with a gradient of 0-35% ethyl acetate in cyclohexane