Reaktion #62557

ord-9a103a7e86b8409ea9662cee16a2dda8

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAfter removing the insoluble material
  2. 2
    Filtrationby filtration
  3. 3
    workup.ADDITIONthe filtrate is diluted with 100 ml of water
  4. 4
    Waschenwashed twice with CH2Cl2
  5. 5
    Extraktionextracted twice with CH2Cl2
  6. 6
    WaschenThe combined organic extracts are washed once with brine
  7. 7
    Trocknendried over MgSO4
  8. 8
    Einengenconcentrated by evaporation

Vorschrift

At 0°, 12 ml of chloroformic acid allyl ester are added dropwise to a solution of 7.51 g of glycine in 20 ml of water and 44 ml of 5N NaOH solution. The suspension is then stirred for 16 hours at room temperature. After removing the insoluble material by filtration, the filtrate is diluted with 100 ml of water and washed twice with CH2Cl2. The aqueous phase is adjusted to pH 2 with 4N HCl and extracted twice with CH2Cl2. The combined organic extracts are washed once with brine, dried over MgSO4 and concentrated by evaporation to form the white crystals of the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04761408uspto-grants-1988_08