反应详情

To a mixture of 3-(2-bromo-4-nitrophenoxy)-4-(difluoromethoxy)benzaldehyde (11.5 g, 0.030 mol) and sodium acetate (3.7 g, 0.045 mol) in dimethylformamide (50 mL) palladium(II) acetate (0.68 g, 0.003 mol) was added in 4 different lots with 1 hour duration at 120-125° C. After the completion of the addition, it was refluxed for 16 hours. The reaction mixture was filtered through hyflo, washed with dimethylformamide (10 mL). The filtrate was poured into the cold water. The solid separated out was filtered. The solid was washed with hexane and dried. Yield—73.3%. HPLC (purity): 84.5%; Rf—0.5 (Ethyl acetate:Hexane (3:7)

1. additionwas added in 4 different lots with 1 hour duration at 120-125° C
2. additionAfter the completion of the addition, it
3. temperaturewas refluxed for 16 hours
4. filtrationThe reaction mixture was filtered through hyflo
5. washwashed with dimethylformamide (10 mL)
6. additionThe filtrate was poured into the cold water
7. customThe solid separated out
8. filtrationwas filtered
9. washThe solid was washed with hexane
10. customdried