反应详情

To a stirring solution of N-[1-(2-benzyloxy-ethyl)-2-oxo-propyl]-4-bromo-2-fluoro-benzamide (1.0 mmol) (See Intermediate 36) in dimethylformamide (0.25M), slowly add phosphorus oxychloride (3.0 mmol) and heat to 90° C. for 2.5 hours. After this time, remove the heat and carefully add water (same amount as DMF) and allow the reaction to cool to room temperature before extracting with ether. Wash organics with water and brine. Dry the organics with sodium sulfate, filter and concentrate in vacuo. Purify via radial chromatography eluting with ethyl acetate and hexane. MS (m/e) (79Br/81Br): 390.2/392.2 (M+1)

1. customAfter this time, remove the
2. temperatureheat
3. customthe reaction
4. extractionbefore extracting with ether
5. dry with materialDry the organics with sodium sulfate
6. filtrationfilter
7. concentrationconcentrate in vacuo
8. customPurify via radial chromatography
9. washeluting with ethyl acetate and hexane