반응 #83740

ord-f3d76ff78a1d49d78bb0dc409b311591

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.DISTILLATIONThe solvent mixture is distilled off
  2. 2
    workup.ADDITIONacetonitrile is added to the oily residue
  3. 3
    여과The crystals which gradually form are filtered off
  4. 4
    세척washed with a small amount of acetonitrile
  5. 5
    기타dried under a high vacuum
  6. 6
    기타[α]D20 =-9.0° (1% in water)

실험 절차

2.07 g of 2(S)-amino-3(S)-carboxy-4(R)-pentanolide are suspended in 10 ml of methanol and dissolved by the addition of 13 ml of 2N aqueous sodium hydroxide solution with stirring at room temperature. The solvent mixture is distilled off and acetonitrile is added to the oily residue. The crystals which gradually form are filtered off, washed with a small amount of acetonitrile and dried under a high vacuum. The disodium salt of the title compound remains behind, [α]D20 =-9.0° (1% in water). 1H-NMR (D2O): 1.21 (3H, d 6.4 Hz), 2.54 (1H, dxd 6.4 and 8.4 Hz), 3.49 (1H, d 6 Hz), 3.97 (1H, dxq 8.4 and 6.4 Hz).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05625059uspto-grants-1997_04