반응 #2021478

ord-cd1897f09e154f11a129d2603cfaff4e

반응 방정식

CC(=O)[O-].[Na+]
sodium acetate
CCN(CCOC(C)=O)c1ccccc1
2-(N-ethylanilino)ethyl acetate
O=P(Cl)(Cl)Cl
phosphoryl chloride
CCN(CCOC(C)=O)c1ccc(C=O)cc1
2-(ethyl(4-formylphenyl)amino)ethyl acetate
수율 84.2%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타to react for 6 hours at room temperature
  2. 2
    추출An organic layer was extracted with ethyl acetate

실험 절차

After adding 55.8 g of ice-cooled phosphoryl chloride to 26.6 g of dimethylformamide, a solution of 63.0 g of the 2-(N-ethylanilino)ethyl acetate in 40 ml of dimethylformamide was slowly added at room temperature, this was caused to react for 6 hours at room temperature while stirring, and then poured into an aqueous solution of 150 g of sodium acetate under ice cooling. An organic layer was extracted with ethyl acetate and the solvent was boiled off under reduced pressure. This was refined by silica gel column chromatography to yield 60.2 g of 2-(ethyl(4-formylphenyl)amino)ethyl acetate.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06383714B1uspto-grants-2002_05