反应详情

At 0° C. SOCl2 (0.88 mmol) is added to a stirred solution of 2-acetylamino-3-(3-fluoro-phenyl)-3-oxo-propionic acid ethyl ester (0.63 mmol) in CHCl3 (0.38 mL). After 30 min the mixture is heated to reflux for 60 min. An additional portion of SOCl2 (0.16 mmol) is added and the mixture is heated to reflux for further 60 min. An aq. K2CO3 solution (1.0 M) is added, the layers are separated and the aq. layer is extracted twice with ether. The combined organic layers are washed with water, dried over MgSO4, filtered and concentrated in vacuo to give the desired ester which is used without further purification. LC-MS: tR=0.93 min; [M+H]+=250.3.

1. customAt 0° C
2. temperatureAfter 30 min the mixture is heated
3. temperatureto reflux for 60 min
4. temperaturethe mixture is heated
5. temperatureto reflux for further 60 min
6. customthe layers are separated
7. extractionthe aq. layer is extracted twice with ether
8. washThe combined organic layers are washed with water
9. dry with materialdried over MgSO4
10. filtrationfiltered
11. concentrationconcentrated in vacuo