Reaktion #7898

ord-5d4e1bbe08d4416ebf8a9bbeacc66b58

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwarmed to room temperature for 24 h
  2. 2
    EinengenConcentration in vacuo
  3. 3
    Sonstigegave a residue which
  4. 4
    Waschenwashed with water, saturated sodium bicarbonate and brine
  5. 5
    SonstigeThe organic layer was separated
  6. 6
    Trocknendried with sodium sulfate
  7. 7
    Filtrationfiltered
  8. 8
    Einengenconcentrated in vacuo

Vorschrift

To a solution of (R)-2-hydroxy-3-phenylpropionic acid (1.5 g, 12.9 mol) in methanol (18 mL) at 0° C. was added concentrated sulfuric acid (0.2 mL). The reaction mixture was stirred at 0° C. for 30 min and warmed to room temperature for 24 h. Concentration in vacuo gave a residue which was diluted with diethyl ether (200 mL) and washed with water, saturated sodium bicarbonate and brine. The organic layer was separated, dried with sodium sulfate, filtered and concentrated in vacuo giving a white solid 1.62 g (85%), which was used without further purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07087622B2uspto-grants-2006_08