反応 #2492360

ord-1c238636c2eb482ab6055672df06a17a

反応方程式

COC(=O)C(C)Oc1ccc(NC(C)=O)cc1
2-(4-acetylamino-phenoxy)-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
63
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
    workup.DISTILLATIONExcess concentrated hydrochloric acid was distilled in vacuum
  2. 2
    ろ過filtered hot
  3. 3
    ろ過filtered
  4. 4
    その他dried

実験手順

To a mixture 2-(4-acetylamino-phenoxy)-propionic acid methyl ester 62 (320 grams, 1.35 mol) in concentrated hydrochloric acid (8 liters) was refluxed for 48 hours. Excess concentrated hydrochloric acid was distilled in vacuum and filtered hot. The mixture was cooled to 10° C., filtered and dried to give pure 63 (240 grams, 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: US08802892B2uspto-grants-2014_08