反応 #54664

ord-d4a83106185d4c60b359d7037c4b05d9

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The reaction mixture becomes warm
  2. 2
    その他finally a yellow oil starts to separate out
  3. 3
    workup.ADDITIONwas poured into water
  4. 4
    その他The organic layer was separated
  5. 5
    洗浄washed with dilute H2SO4
  6. 6
    乾燥dried (MgSO4)
  7. 7
    その他Removal of the solvent
  8. 8
    workup.WAITleft a viscous oil (3.8 g.)
  9. 9
    workup.DISTILLATIONThis was distilled under vacuum

実験手順

A solution of p-menth-3-oyl chloride prepared as in Example 1 (4.0g., 0.020 moles) in chloroform (30 ml.) was added dropwise to a stirred solution of ethanolamine (3 g., 0.043 moles) in chloroform (50 ml.). The reaction mixture becomes warm, goes cloudy and finally a yellow oil starts to separate out. After stirring for 2 hours at room temperature the mixture was poured into water. The organic layer was separated, washed with dilute H2SO4, and dried (MgSO4). Removal of the solvent left a viscous oil (3.8 g.). This was distilled under vacuum to yield N-(2-hydroxyethyl)-p-menthane-3-carboxamide as a colourless very viscous oil, b.p. 160°/01. mm.

出典

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