反应详情

温度

250 °C

3.7 g (2.3 mmol) of N-acetyl-m-anisidine, 10.6 g (41.4 mmol) of 4-bromo-N,N-diethylbenzamide and 0.42 g of CuI were heated to 1000° C.; 3 g (22.3 mmol) of K2CO3 were added and the resulting mixture was heated to 250° C. for 2 hours. The residue was dissolved in CH2Cl2 and washed with H2O, the organic layer was dried over Na2SO4 and the solvent was removed in vacuo. The resulting residue was dissolved in 20 ml of absolute EtOH and refluxed for 2 h. The solvent was removed in vacuo, the residue was taken up in H2O and the aqueous layer extracted with AcOEt. The organic layer was dried over Na2SO4 and the solvent removed in vacuo. The resulting residue was purified by flash chromatography (AcOEt/Hexane 6:4), yielding 3 g of the title compound.

1. washwashed with H2O
2. dry with materialthe organic layer was dried over Na2SO4
3. customthe solvent was removed in vacuo
4. dissolutionThe resulting residue was dissolved in 20 ml of absolute EtOH
5. temperaturerefluxed for 2 h
6. customThe solvent was removed in vacuo
7. extractionthe aqueous layer extracted with AcOEt
8. dry with materialThe organic layer was dried over Na2SO4
9. customthe solvent removed in vacuo
10. customThe resulting residue was purified by flash chromatography (AcOEt/Hexane 6:4)