反応 #1969493

ord-82cbff6014224e91ba986ac18a5b1551

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: US08318973B2uspto-grants-2012_11