反応 #470995

反応方程式

3-bromo-2-hydroxybenzaldehyde

2-chloro-N,N-dimethylacetamide

potassium carbonate

→

title compound

収率 99.4%

7-Bromo-N,N-dimethyl-benzofuran-2-carboxamide

収率 99.4%

溶媒

DMF

反応条件

後処理

1. 1
   温度was heated
2. 2
   温度at reflux for 1 h
3. 3
   ろ過The solids were filtered off
4. 4
   濃縮the filtrate was concentrated
5. 5
   洗浄washed with sat. NaCl(aq)
6. 6
   その他The layers were separated
7. 7
   抽出the aqueous layer was extracted with ethyl acetate (2×50 mL)
8. 8
   乾燥The combined organic layer was dried with sodium sulfate
9. 9
   ろ過filtered
10. 10
    濃縮concentrated

実験手順

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.

出典