Reaktion #65737

Reaktionsgleichung

acetic anhydride

sodium formate

Phenylglycine ethyl ester hydrochloride

acetic anhydride

→

N-Formylphenylglycine ethyl ester

Lösungsmittel

formic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGthe mixture was stirred at 50°-60° C. for 1.5 hours
2. 2
   workup.DISTILLATIONAfter the solvent was distilled off
3. 3
   Extraktionextracted with ethyl acetate
4. 4
   WaschenThe organic layer was washed with a saturated aqueous solution of sodium chloride
5. 5
   Trocknendried over magnesium sulfate
6. 6
   workup.DISTILLATIONThe solvent was distilled off
7. 7
   Sonstigeto afford an oily product

Vorschrift

Phenylglycine ethyl ester hydrochloride (21.5 g; 0.1 mol) was dissolved in 200 ml of formic acid, whereto sodium formate (8.16 g; 1.2 eq.) was added, followed by adding dropwise acetic anhydride (20 ml; 2.1 eq.). After two hours' stirring, 10 ml of acetic anhydride was added dropwise, and the mixture was stirred at 50°-60° C. for 1.5 hours. After the solvent was distilled off, the residue was neutralized with an aqueous solution of sodium hydrogencarbonate and extracted with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium chloride and dried over magnesium sulfate. The solvent was distilled off to afford an oily product.

Quelle