반응 #725888

ord-f28df230f2a842f6bd81173f55feb8ca

반응 방정식

CCOC(=O)COc1ccc(NC(C)=O)cc1
(4-Acetylamino-phenoxy)-acetic acid ethyl ester
Cl
hydrochloric acid
Cl.Nc1ccc(OCC(=O)O)cc1
14
수율 77.6%
Cl.Nc1ccc(OCC(=O)O)cc1
(4-Amino-phenoxy) acetic acid HCl
수율 77.6%

반응 조건

온도
10°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.DISTILLATIONExcess concentrated hydrochloric acid was distilled off in vacuum
  2. 2
    여과filtered hot
  3. 3
    여과filtered
  4. 4
    기타dried

실험 절차

A mixture (4-Acetylamino-phenoxy)-acetic acid ethyl ester 13 (375 g, 1.582 mmol), in concentrated hydrochloric acid (9.36 liters) was refluxed for 12 hours. Excess concentrated hydrochloric acid was distilled off in vacuum and filtered hot. The mixture was cooled to 10° C., filtered and dried to give pure 14 (250 g, 77.6%) as a wheat colored powder. The melting point was found to be 224-226° C. The structure was confirmed with NMR.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07691364B2uspto-grants-2010_04