反应详情

温度

77.5 °C

To a mixture of 3-Benzyloxy-4-hydroxy benzaldehyde (15 g, 0.065 mol) and Iodine (17.54 g, 0.13 mol) was added 3.2% NaOH solution (150 ml). The reaction mixture was stirred at 75-80° C. for 8 h. The reaction mixture was cooled to room temperature and concentrated hydrochloric acid was added and the solid was filtered. Then the compound was recrystalized with isopropanol. The solid was filtered and dried to give 3-benzyloxy-4hydroxy-5-Iodo benzaldehyde (18.40 g, 79%). TLC: Ethyl acetate:light petroleum (2:5), Rf=0.4; 1H NMR (CDCl3, 200 MHz): δ 5.20 (s, 2H), 7.23-7.45 (m, 6H), 7.8 (d, J=1.42 Hz, 1H), 9.73 (s,1H).

1. temperatureThe reaction mixture was cooled to room temperature
2. filtrationthe solid was filtered
3. customThen the compound was recrystalized with isopropanol
4. filtrationThe solid was filtered
5. customdried