반응 #1741369

ord-c8581ffa6e69462b89d459cd128f7ce9

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONto which was added, under ice-
  2. 2
    온도cooling
  3. 3
    온도The reaction mixture was cooled with ice, to which
  4. 4
    추출followed by extraction with dichloromethane (200 ml) three times
  5. 5
    세척washed with a saturated aqueous saline solution (100 ml) twice
  6. 6
    건조by drying over anhydrous magnesium sulfate
  7. 7
    workup.DISTILLATIONThe solvent was distilled off under reduced pressure

실험 절차

In ethanol (450 ml) was dissolved ethyl(2S)-2-(3,4,5,6-tetrahydro-2H-pyran-2-yloxy)propionate, to which was added, under ice-cooling, 2N sodium hydroxide solution (150 ml), and the mixture was stirred for one hour at room temperature. The reaction mixture was cooled with ice, to which was added a 27° C. aqueous solution of acetic acid (100 ml), followed by extraction with dichloromethane (200 ml) three times. Dichloromethane layers were combined and washed with a saturated aqueous saline solution (100 ml) twice, followed by drying over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to leave (2S)-2-(3,4,5,6-tetrahydro-2H-pyran-2-yloxy)propionic acid (29.5 g) as a colorless waxy product.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05405861uspto-grants-1995_04