反応 #2045007

ord-9aba51634b83439c8b305fedd0029c86

反応方程式

COC(=O)C(C)Oc1ccc(NC(C)=O)cc1
2-(4-Acetylaminophenoxy)propionic acid methyl ester
COC(=O)C(C)Oc1ccc(NC(C)=O)cc1
2-(4-Acetylamino-phenoxy)-propionic acid methyl ester
CC(Oc1ccc(N)cc1)C(=O)O
17
収率 98.1%
CC(Oc1ccc(N)cc1)C(=O)O
2-(4-Amino-phenoxy)-propionic acid
収率 98.1%

反応条件

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

後処理

  1. 1
    温度was refluxed for 48 hours
  2. 2
    workup.DISTILLATIONExcess concentrated hydrochloric acid was distilled off in vacuum
  3. 3
    ろ過filtered hot
  4. 4
    ろ過filtered
  5. 5
    その他dried

実験手順

A mixture of 2-(4-Acetylaminophenoxy)propionic acid methyl ester 16 (320 grams, 1.35 mol) in concentrated hydrochloric acid (8 liters) was refluxed for 48 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 17 (240 g, 81.7%) as a brown powder. The melting point was found to be 175-180° C.

出典

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