Reaktion #90850

ord-3c91b85feed141eba2da4cf9e8233326

Reagenzien

Keine

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction mixture was refluxed for 15 hours
  2. 2
    SonstigeEvaporation of the reaction mixture under reduced pressure
  3. 3
    Sonstigefollowed by crystallization of the resulting residue from methanol and methyl tert-butyl ether

Vorschrift

D-serine (100 g, 0.9515 mole) was suspended in 600 ml methanol at room temperature. Acetyl chloride (224.0 g, 2.8545 mole) was added drop wise at −5° C. to 0° C. and stirred for 30 minutes. The reaction mixture was refluxed for 15 hours. Evaporation of the reaction mixture under reduced pressure followed by crystallization of the resulting residue from methanol and methyl tert-butyl ether, resulted in colorless solid of D-serine methyl ester hydrochloride (134.7 g, Yield: 91%, HPLC: 99.6%)

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09447024B1uspto-grants-2016_09