反応 #2045004

ord-38f5b847ce1f4af9b1d105bee75bf64b

反応方程式

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

反応条件

温度
10°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.DISTILLATIONExcess concentrated hydrochloric acid was distilled off in vacuum
  2. 2
    ろ過filtered hot
  3. 3
    ろ過filtered
  4. 4
    その他dried

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08409559B2uspto-grants-2013_04