반응 #64869

ord-6799667dd05d48d48fc66659400e1725

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도is heated
  2. 2
    온도under reflux for 6 h
  3. 3
    농축Then the reaction mixture is concentrated in vacuo
  4. 4
    workup.ADDITIONdiluted with water (50 ml)
  5. 5
    세척washed twice with ether (100 ml)
  6. 6
    workup.ADDITIONThen the aqueous solution is poured on an ion exchange resin column (DOWEX 50, H+) The column
  7. 7
    세척is eluted with 1M ammonium hydroxide

실험 절차

A mixture of glyoxylic acid monohydrate (23 g, 250 mmol), propargyl alcohol (16.8 g, 300 mmol ), copper (II) chloride (3.2 g, 25 mmol) and ammonium acetate (49 g, 600 mmol) in ethanol (100 ml) is heated under reflux for 6 h. Then the reaction mixture is concentrated in vacuo, diluted with water (50 ml), acidified to pH 5 with 1N HCl and washed twice with ether (100 ml). Then the aqueous solution is poured on an ion exchange resin column (DOWEX 50, H+) The column is eluted with 1M ammonium hydroxide to give the title compound 2-amino-5-hydroxy-3-pentynoic acid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05416076uspto-grants-1995_05