Acetic Anhydride → ethyl 2-(N-phenylformamido)acetate

HRID 37459ノート

反応式

HRID 37459 の反応式
Cl.[CH2:2]([O:4][C:5](=[O:14])[CH2:6][NH:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[CH3:3].[CH:15]([O-])=[O:16].[Na+].C(OC(=O)C)(=O)C>C(O)=O>[CH2:2]([O:4][C:5](=[O:14])[CH2:6][N:7]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[CH:15]=[O:16])[CH3:3]

参加物

5

反応物 3

HCID 7918Acetic Anhydride2 回HCID 2723810Sodium FormateHCID 12241367Ethyl N-phenylglycinate hydrochloride

生成物 1

HCID 14416604ethyl 2-(N-phenylformamido)acetate

試薬・触媒・溶媒 1

HCID 284Formic Acid溶媒

実験手順

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.

後処理

  1. stirringthe mixture was stirred at 50°-60° C. for 1.5 hours
  2. distillationAfter the solvent was distilled off
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed with a saturated aqueous solution of sodium chloride
  5. dry with materialdried over magnesium sulfate
  6. distillationThe solvent was distilled off
  7. customto afford an oily product

出典と根拠

ORDレコード
ord-512e925bfd144f51b8b4b5a983f7a023
出典データセット
uspto-grants-1995_05
特許番号
US05420275

反応ノート

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