反应详情

7-Amino-4-(4-hydroxy-3-methoxyphenyl)isoindolinone (50.0 mg, 0.185 mmol) was dissolved in acetonitrile (2.5 mL), and the solution was added with tert-butyldimethylsilyl chloride (33.5 mg, 0.222 mmol), 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU) (0.033 mL, 0.22 mmol), followed by stirring at room temperature for 1.3 hours. The mixture was added with tert-butyldimethylsilyl chloride (33.5 mg, 0.222 mmol) and DBU (0.033 mL, 0.22 mmol), followed by further stirring for 1 hour. The reaction mixture was added with water and extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by preparative thin-layer chromatography (chloroform/acetonitrile=2/1) to obtain 7-amino-4-(4-tert-butyldimethylsilyloxy-3-methoxyphenyl)isoindolinone (51.1 mg, yield 72%).

1. stirringby further stirring for 1 hour
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed with saturated brine
4. dry with materialdried over anhydrous sodium sulfate
5. customThe solvent was evaporated under reduced pressure
6. customthe residue was purified by preparative thin-layer chromatography (chloroform/acetonitrile=2/1)