反应详情

温度

50 °C

To a suspension of 1.4 g (4.3 mmol) N-[2-(4-Methoxy-phenyl)-2-oxo-ethyl]-isophthalamic acid methylester from Preparation 2 in 30 mL of dry dioxane was added 1.1 g (5.2 mmol) of P2S5 in one portion. The resulting mixture was warmed to 50° C. for 1 hour before cooling to room temperature and adding about 60 ml water. Stirred 2 hours and then filtered off solid product. Triturated in hot MeOH and filtered. Dissolved in THF and filtered through a plug of flash silica gel with THF eluent. Concentration gave 1.4 g (100%) of desired product. Used directly in the procedure of Preparation 11 without characterization.

1. temperaturebefore cooling to room temperature
2. filtrationfiltered off solid product
3. customTriturated in hot MeOH
4. filtrationfiltered
5. dissolutionDissolved in THF
6. filtrationfiltered through a plug of flash silica gel with THF eluent
7. concentrationConcentration