تفاعل #65737

ord-512e925bfd144f51b8b4b5a983f7a023

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  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
    استخلاصextracted with ethyl acetate
  4. 4
    غسيلThe organic layer was washed with a saturated aqueous solution of sodium chloride
  5. 5
    تجفيفdried over magnesium sulfate
  6. 6
    workup.DISTILLATIONThe solvent was distilled off
  7. 7
    أخرىto afford an oily product

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05420275uspto-grants-1995_05