Реакция #2045004

ord-38f5b847ce1f4af9b1d105bee75bf64b

Уравнение реакции

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

Условия реакции

Температура
10°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

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

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08409559B2uspto-grants-2013_04