反应详情

2-tert-Butyl-7-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-6-(3-methoxyphenyl)-5-methyl-1,3-benzoxazole-4-carbonitrile (I-23) (10 mg, 23.1 μmol) was dissolved (partially suspended) in benzene (2.0 ml), and dropwise added to a benzene (2.0 ml) suspension reflux liquid of aluminium chloride (9.2 mg, 69.0 μmol). The benzene wash (8.0 ml) of the eggplant-type flask with the starting material adhering thereto was also added, followed by refluxing for 0.5 hours. After cooling, aluminium chloride (61.7 mg, 462 μmol) was further added, followed by further stirring under reflux for 15 minutes. After cooling, saturated sodium bicarbonate water (50 ml) was added to the reaction liquid, the product was extracted with chloroform (50 ml×2), ethyl acetate (50 ml).

1. washThe benzene wash (8.0 ml) of the eggplant-type flask with the starting material adhering
2. additionthereto was also added
3. temperatureby refluxing for 0.5 hours
4. temperatureAfter cooling
5. temperatureunder reflux for 15 minutes
6. temperatureAfter cooling
7. extractionthe product was extracted with chloroform (50 ml×2), ethyl acetate (50 ml)