反应详情

A solution of 2-chloro-N-(3-fluoro-2-methylphenyl)acetamide (47.2 g, 234 mmol) in conc. sulphuric acid (220 ml) was treated at ca. −20° C. (ethanol/water/CO2(s) bath) with conc. nitric acid (69%, 15.25 ml, 19 g, 235 mmol) over 30 minutes, keeping internal temperature ≦9° C. The reaction was complete at the end of the addition. The mixture was added to ice with vigorous stirring then left to stand overnight. Filtration, washing of the solid with water and drying afforded the product (54.6 g, 95%) containing ˜9% impurity.

1. customtemperature ≦9° C
2. additionThe reaction was complete at the end of the addition
3. additionThe mixture was added to ice
4. waitthen left
5. filtrationFiltration
6. washwashing of the solid with water
7. customdrying