反应详情

Et3N (8.88 ml) was added to a solution of 2-amino-1-(4-nitrophenyl)ethanone hydrochloride (step B product, 11.5 g) in EtOAc (115 ml). This was followed by drop wise addition of Ethylchlorooxoacetate (7.11 ml). The reaction mixture was refluxed for 2 hours. It was then cooled and quenched with water. The organic layer was separated, dried over Na2SO4 and the solvent was concentrated to get dark brown oil which was purified by column chromatography in 3:7 Ethyl acetate:Pet ether to get yellow solid. The solid was crystallized in ethyl acetate/pet ether to yield 8.9 g (59%) of the title compound. 1HNMR (DMSO-d6, 300 MHz): δ 9.21 (t, 1H), 8.35 (d, 2H), 8.24 (d, 2H), 4.78 (d, 2H), 4.29 (q, 2H), 1.29 (t, 3H).

1. temperatureThe reaction mixture was refluxed for 2 hours
2. temperatureIt was then cooled
3. customquenched with water
4. customThe organic layer was separated
5. dry with materialdried over Na2SO4
6. concentrationthe solvent was concentrated
7. customto get dark brown oil which
8. customwas purified by column chromatography in 3:7 Ethyl acetate
9. customPet ether to get yellow solid
10. customThe solid was crystallized in ethyl acetate/pet ether