反应详情

温度

27.5 °C

To a stirred solution of phthalimide (0.6 g, 4.0 mmol) in DMF (5 ml) was added K2CO3 (2.25 g, 16.00 mmol), followed by 4-iodobenzyl bromide (1.33 g, 4.4 mmol) at 0° C. and the reaction mixture was stirred at 20-35° C. for 16 h. The progress of the reaction was monitored by TLC. After 16 h of stirring, the mixture was diluted with water (50 ml) and extracted with ethyl acetate (2×50 ml). The combined organic layers were washed with brine (50 ml), followed by drying over anhydrous Na2SO4 and filtering. The filtrate was rotary evaporated to get residue which was washed with diethyl ether to get the desired compound as a white solid (700 mg, 50%). 1H NMR (400 MHz, DMSO-d6) δ 7.91-7.84 (m, 4H), 7.70-7.66 (m, 2H), 7.12 (d, J=8.3 Hz, 2H), 4.72 (s, 2H).

1. stirringAfter 16 h of stirring
2. extractionextracted with ethyl acetate (2×50 ml)
3. washThe combined organic layers were washed with brine (50 ml)
4. dry with materialby drying over anhydrous Na2SO4
5. filtrationfiltering
6. customThe filtrate was rotary evaporated
7. customto get residue which
8. washwas washed with diethyl ether