反应详情

A solution of 3-(2-methylphenyl)-6,7-dihydro-5H-indeno[5,6-b]furan-2-carboxylic acid (3 g), triethylamine (2.2 ml) and DPPA (2.9 ml) in benzene (200 ml) was stirred at room temperature for 1 hour, and then heated under reflux for 1 hour. After cooling to room temperature, to the reaction solution 2,6-dimethoxyaniline (1.6 g) was added and then heated under reflux for 1 hour. The reaction solution was combined with water and chloroform, and the organic layer was washed with diluted hydrochloric acid followed by a saturated aqueous solution of sodium hydrogen carbonate and water, and after drying over magnesium sulfate, the solvent was distilled off under reduced pressure. The resultant residue was purified by a silica gel column chromatography (eluent: chloroform), and further purified by recrystallization from THF-chloroform to obtain the title compound as a colorless crystal (2.4 g, 53%).

1. temperatureheated
2. temperatureunder reflux for 1 hour
3. additionwas added
4. temperatureheated
5. temperatureunder reflux for 1 hour
6. washthe organic layer was washed with diluted hydrochloric acid
7. dry with materialafter drying over magnesium sulfate
8. distillationthe solvent was distilled off under reduced pressure
9. customThe resultant residue was purified by a silica gel column chromatography (eluent: chloroform)
10. customfurther purified by recrystallization from THF-chloroform