반응 #65737

ord-512e925bfd144f51b8b4b5a983f7a023

반응 방정식

CC(=O)OC(C)=O
acetic anhydride
O=C[O-].[Na+]
sodium formate
CCOC(=O)CNc1ccccc1.Cl
Phenylglycine ethyl ester hydrochloride
CC(=O)OC(C)=O
acetic anhydride
CCOC(=O)CN(C=O)c1ccccc1
N-Formylphenylglycine ethyl ester

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  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
    추출extracted with ethyl acetate
  4. 4
    세척The organic layer was washed with a saturated aqueous solution of sodium chloride
  5. 5
    건조dried over magnesium sulfate
  6. 6
    workup.DISTILLATIONThe solvent was distilled off
  7. 7
    기타to afford an oily product

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05420275uspto-grants-1995_05