反应详情

Into a 1000-mL round-bottom flask, was placed a solution of 4-bromo-2-fluorobenzoic acid (50 g, 229.36 mmol, 1.00 equiv) in dichloromethane (600 mL), N-methoxymethanamine hydrochloride (25 g, 257.73 mmol, 1.10 equiv). To the resulting mixture was added DIC (32 g, 253.97 mmol, 1.10 equiv) at 0° C. The resulting solution was stirred for 4 h at room temperature. The reaction was then quenched by the addition of water (500 mL). The solids were filtered out. The resulting solution was extracted with DCM (2×300 mL) and the organic layers combined. The resulting mixture was washed with water (2×300 mL), and sodium carbonate (1×300 mL). The resulting mixture was washed with brine (1×300 mL), then dried over anhydrous sodium sulfate and concentrated under vacuum to yield 4-bromo-2-fluoro-N-methoxy-N-methylbenzamide as colorless oil.

1. customInto a 1000-mL round-bottom flask, was placed
2. customThe reaction was then quenched by the addition of water (500 mL)
3. filtrationThe solids were filtered out
4. extractionThe resulting solution was extracted with DCM (2×300 mL)
5. washThe resulting mixture was washed with water (2×300 mL), and sodium carbonate (1×300 mL)
6. washThe resulting mixture was washed with brine (1×300 mL)
7. dry with materialdried over anhydrous sodium sulfate
8. concentrationconcentrated under vacuum