반응 #4224

ord-aa9ed74e9a0d49428bacce5162b0c162

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was heated at its boiling point for 15 minutes
  2. 2
    workup.DISTILLATIONAfter some of the solvent had been distilled off
  3. 3
    기타the product precipitated
  4. 4
    여과thereby was suction-filtered off

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04723989uspto-grants-1988_02