反应详情

In 20 ml of methylene chloride, 1.20 g of 1,2,3,4,5,6-hexahydrophthalic acid monoethyl ester was dissolved. To this solution 0.47 g of pyridine and 0.71 g of thionyl chloride were added and the resulting mixture was stirred at room temperature. Two hour later, 1 20 g of 5-allyloxy-4-chloro-2-fluoroaniline and 0.61 g of triethylamine were added and the resulting mixture was stirred at room temperature for 5 hours. After completion of the reaction, 10% hydrochloric acid was added to the reaction mixture to make the same acidic and was extracted twice with methylene chloride. The extract was washed with saturated aqueous sodium hydrogen carbonate and dried over magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by column chromatography (silica gel, hexane/ethyl acetate =5/1 (v/v)) to obtain 1.5 g of light brown crystal.

1. stirringthe resulting mixture was stirred at room temperature for 5 hours
2. additionwas added to the reaction mixture
3. extractionwas extracted twice with methylene chloride
4. washThe extract was washed with saturated aqueous sodium hydrogen carbonate
5. dry with materialdried over magnesium sulfate
6. customThe solvent was evaporated under reduced pressure
7. customthe residue was purified by column chromatography (silica gel, hexane/ethyl acetate =5/1 (v/v))