反応 #54663

ord-1d94e2ec81454ab69745a7f772ddee44

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他At the end of this time the ether layer was separated
  2. 2
    乾燥dried (MgSO4)
  3. 3
    その他Removal of the solvent
  4. 4
    workup.WAITleft an oily solid (12.3 g.)
  5. 5
    workup.DISTILLATIONThis was distilled under reduced pressure

実験手順

Sodium bicarbonate (8.4 g., 0.1 mole) and glycine ethyl ester hydrochloride (7 g. 0.05 mole) were dissolved in water (100 ml.), and a solution of p-menth-3-oyl chloride (10 g., 0.05 mole) in ether (50 ml.) was added and the mixture stirred vigorously at room temperature for 2 hours. At the end of this time the ether layer was separated and dried (MgSO4). Removal of the solvent left an oily solid (12.3 g.). This was distilled under reduced pressure to yield N-p-menth-3-oylglycine ethyl ester, bp. 150- 2°/0.1 mm. as a colourless liquid which rapidly solidified.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04150052uspto-grants-1979_04