2,3-二氢-5-碘-1H-异吲哚-1-酮

反应条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a suspension of 5-iodo-2,3-dihydroisoindol-1-one (3 g) in DMF (60 mL), were added N,N-dimethylaminopyridine (DMAP: 14 mg), Et3N (4.84 mL) and tert-butyl-diphenylsilyl chloride (9.0 mL). The mixture was stirred at 50° C. for 2 h. After cooling, saturated NaHCO3 aq. was added into the reaction mixture. Then it was extracted with EtOAc. The organic layer was washed with water and brine, then was dried over anhydrous Na2SO4. The solvent was removed under reduced pressure. The trituration with Et2O followed by filtration gave compound aa2-1 (2.78 g) as a yellow amorphous solid. After cooling Then it was extracted with EtOAc The organic layer was washed with water and brine was dried over anhydrous Na2SO4 The solvent was removed under reduced pressure The trituration with Et2O followed by filtration gave compound aa2-1 (2.78 g) as a yellow amorphous solid

反应条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a suspension of 5-iodo-2,3-dihydroisoindol-1-one (3 g) in DMF (60 mL), were added N,N-dimethylaminopyridine (DMAP: 14 mg), Et3N (4.84 mL) and tert-butyl-diphenylsilyl chloride (9.0 mL). The mixture was stirred at 50° C. for 2 h. After cooling, saturated NaHCO3 aq. was added into the reaction mixture. Then it was extracted with EtOAc. The organic layer was washed with water and brine, then was dried over anhydrous Na2SO4. The solvent was removed under reduced pressure. The trituration with Et2O followed by filtration gave compound aa2-1 (2.78 g) as a yellow amorphous solid. After cooling Then it was extracted with EtOAc The organic layer was washed with water and brine was dried over anhydrous Na2SO4 The solvent was removed under reduced pressure The trituration with Et2O followed by filtration gave compound aa2-1 (2.78 g) as a yellow amorphous solid