反应详情

A mixture of 3-bromo-2-hydroxybenzaldehyde (5 g, 24.87 mmol), 2-chloro-N,N-dimethylacetamide (3.33 ml, 32.34 mmol) and potassium carbonate (6.88 g, 49.75 mmol) in DMF (60 ml) was heated at reflux for 1 h. The solids were filtered off and the filtrate was concentrated. The residue was taken up in ethyl acetate and washed with sat. NaCl(aq). The layers were separated and the aqueous layer was extracted with ethyl acetate (2×50 mL). The combined organic layer was dried with sodium sulfate, filtered and concentrated to give the title compound (6.63 g, 99%) as a crude product which was used as such in subsequent reaction.

1. temperaturewas heated
2. temperatureat reflux for 1 h
3. filtrationThe solids were filtered off
4. concentrationthe filtrate was concentrated
5. washwashed with sat. NaCl(aq)
6. customThe layers were separated
7. extractionthe aqueous layer was extracted with ethyl acetate (2×50 mL)
8. dry with materialThe combined organic layer was dried with sodium sulfate
9. filtrationfiltered
10. concentrationconcentrated