反应详情

To a suspension of NaH (493 g, 12.3 mmol) in DMF (10 ml) was added a solution of 4-aminophthalimide (2.00 g, 12.3 mmol) in DMF (10 ml) at 0° C. After stirring at room temperature for 1 h, iodopropane (1.20 ml, 12.3 mmol) was added to this mixture at 0° C. and stirred at room temperature for 28 h. The mixture was poured into water and extracted with AcOEt:toluene=2:1 (150 ml×3). The extract was washed with water, brine, dried (Na2SO4), and concentrated to give yellow solid, which was purified by column chromatography (silica gel: 130 g, CH2Cl2 only to CH2Cl2/MeOH=75/1) to give 1.14 g (45%) of yellow solid.

1. stirringstirred at room temperature for 28 h
2. extractionextracted with AcOEt
3. washThe extract was washed with water, brine
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated
6. customto give yellow solid, which
7. customwas purified by column chromatography (silica gel