反应详情

温度

40 °C

A solution of sodium hypobromite, prepared at 0° C. by dissolving sodium hydroxide (45.71 g, 1.14 mole) in water (200 mL) and bromine (16.3 mL, 0.30 mole) over 5 minutes. This solution is then added dropwise over 30 minutes to a solution of 1-[2-methyl-4-(2-morpholin-4-yl-ethoxy)-phenyl]-ethanone (19.2 g, 0.073 mole) in dioxane (140 mL), then warmed to 40° C. and stirred for 30 minutes. Sodium bisulfite is added to destroy the excess sodium hypobromite and then diluted with water (800 mL) and stirred overnight at ambient temperature. The volume is reduced in-vacuo by about 300 mL and then acidified with 3 N hydrochloric acid to pH 6. This is then extracted repeatedly with ethyl acetate. The combined organic layers were dried over sodium sulfate, filtered and evaporated to give a white solid, 4.09 g (21%), MS (ESI): m/z 266.2 (M+H).

1. customto destroy the excess sodium hypobromite
2. additiondiluted with water (800 mL)
3. stirringstirred overnight at ambient temperature
4. extractionThis is then extracted repeatedly with ethyl acetate
5. dry with materialThe combined organic layers were dried over sodium sulfate
6. filtrationfiltered
7. customevaporated
8. customto give a white solid, 4.09 g (21%), MS (ESI)