反応 #4224

ord-aa9ed74e9a0d49428bacce5162b0c162

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度was heated at its boiling point for 15 minutes
  2. 2
    workup.DISTILLATIONAfter some of the solvent had been distilled off
  3. 3
    その他the product precipitated
  4. 4
    ろ過thereby was suction-filtered off

実験手順

A mixture of 46 g of dimethylmaleic acid anhydride, 48 g of 2-amino-2,3-dimethylbutyric acid amide and 70 ml of methylene chloride was heated at its boiling point for 15 minutes. After some of the solvent had been distilled off, the residual mixture was stirred with 300 ml of diethyl ether, and the product precipitated thereby was suction-filtered off. The desired compound (II) (90 g; 96%) was isolated as a crystalline solid, melting point 70°-72° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04723989uspto-grants-1988_02