反应详情

A mixture of 4-aminosulfonyl-2-carbamoylmethoxyphenoxyacetamide (Intermediate A66, 12.1 g, 0.040 mol), potassium carbonate (11.0 g, 0.80 mol), and dimethylacetamide (160 mL) was heated at reflux as 3-fluoro-4-nitroanisole (6.84 g, 0.040 mol) in 40 mL dimethylacetamide was added dropwise over 40 min. After an additional 30 min at reflux, the mixture was allowed to cool overnight. It was then diluted with 200 mL of water and filtered with the aid of additional water. The filtrate was brought to pH 5, and the resulting solid was collected and washed with water. After air-drying, the product, title compound weighed 15 g (80%).

1. temperaturewas heated
2. additionwas added dropwise over 40 min
3. temperatureAfter an additional 30 min at reflux
4. temperatureto cool overnight
5. filtrationfiltered with the aid of additional water
6. customthe resulting solid was collected
7. washwashed with water
8. customAfter air-drying