反应详情

温度

100 °C

A mixture of 2-chloro-5-fluoro-6-(methyloxy)-3-pyridinecarboxylic acid (32.65 g, 159 mmol) in toluene/triethylamine/tert-butanol (300 ml/26.4 ml/75 ml) was treated with diphenylphosphoryl azide (37.7 ml, 174.8 mmol) and heated to 100° C. for 2 hours. The mixture was treated with saturated aqueous sodium bicarbonate solution (500 ml) then extracted with ethyl acetate (3×500 ml). The combined organic extracts were dried over magnesium sulphate and evaporated. The residue was chromatographed eluting with 0-40% dichloromethane in petrol affording the product as a white solid (36.35 g, 83%).

1. extractionthen extracted with ethyl acetate (3×500 ml)
2. dry with materialThe combined organic extracts were dried over magnesium sulphate
3. customevaporated
4. customThe residue was chromatographed
5. washeluting with 0-40% dichloromethane in petrol affording the product as a white solid (36.35 g, 83%)