反応 #46917

反応方程式

2,4′-dibromoacetophenone

ethyl acetoacetate

potassium carbonate

→

title compound

ethyl 2-acetyl-4-(4-bromophenyl)-4-oxobutanoate

溶媒

2-butanone

反応条件

後処理

1. 1
   温度at reflux for 24 hours
2. 2
   温度Upon cooling
3. 3
   ろ過the mixture was filtered over diatomaceous earth
4. 4
   濃縮concentrated
5. 5
   その他The residue was purified by chromatography with DCM

実験手順

A mixture of 2,4′-dibromoacetophenone (3.0 g, 10.8 mmol), ethyl acetoacetate (1.48 mL, 10.8 mmol) and potassium carbonate (4.5 g, 32.4 mmol) were heated in 2-butanone (50 mL) at reflux for 24 hours. Upon cooling, the mixture was filtered over diatomaceous earth and concentrated. The residue was purified by chromatography with DCM to provide the title compound as an oil. 1H NMR (CDCl3) δ ppm 1.30 (3H), 2.10 (3H), 3.19 (2H), 3.75 (1H), 4.15 (2H), 7.50 (2H), 7.81 (2H); MS (ESI) m/z 326/328.

出典