反応 #49187

ord-83d523f1f3ab4c6cb52549770aa930ad

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他was ascertained by TLC (19 h)
  2. 2
    その他After 19 h which it was partitioned with dichloromethane (3×100 mL)
  3. 3
    乾燥The organic layer was dried with anhydrous sodium sulfate
  4. 4
    ろ過filtered
  5. 5
    その他evaporated
  6. 6
    workup.DISTILLATIONThe residue was distilled

実験手順

Referring to scheme 16, a 4.7M aqueous solution of sodium hydroxide (50 mL) was added into a stirred, ice-cooled solution of ethyl glycinate hydrochloride (32.19 g, 0.23 mole) in water (50 mL). Then, ethyl acrylate (23.1 g, 0.23 mole) was added and the mixture was stirred at room temperature until the completion of reaction was ascertained by TLC (19 h). After 19 h which it was partitioned with dichloromethane (3×100 mL). The organic layer was dried with anhydrous sodium sulfate, filtered and evaporated. The residue was distilled to afford 58 (28.8 g, 61%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07745608B2uspto-grants-2010_06