反应详情

温度

100 °C

A mixture of dimethyl[3-fluoro-6-(methyloxy)-1,5-naphthyridin-4-yl]propanedioate (52 g, 169 mmol), lithium chloride (14.5 g, 340 mmol) and water (3.43 ml, 190 mmol) in DMSO (1175 ml) was heated at 100° C. for 24 hours and cooled. The solution was shaken with water and ethyl acetate, separated and the organic phase washed twice with water. The total aqueous was re-extracted with ethyl acetate and this water-washed. The combined organic phase was dried and evaporated and the residue chromatographed, using a hexane/ethyl acetate gradient, to give the desired product containing about 10% of starting material (35.79 g).

1. temperaturecooled
2. customseparated
3. washthe organic phase washed twice with water
4. extractionThe total aqueous was re-extracted with ethyl acetate
5. washthis water-washed
6. customThe combined organic phase was dried
7. customevaporated
8. customthe residue chromatographed