반응 #81641

ord-f419fd2893ef45fb8f0259106ff5352c

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타subsequently the reaction liquid
  2. 2
    workup.DISTILLATIONwas distilled by a conventional method
  3. 3
    기타As a result, methyl formate and methanol were recovered

실험 절차

A one L stainless steel-made autoclave equipped with a stirrer was charged with 72.5 g of the methyl 3-carbamoylisobutyrate which had been obtained in the preceding item (2), 180 g of methyl formate, 96 g of methanol and 1.1 g of sodium methylate to proceed with heating reaction at 60° C. for 2 hours. The reaction product was cooled and then analyzed. As a result, the conversion of the methyl 3-carbamoylisobutyrate was 83.2% and, there were obtained dimethyl methylsuccinate at a selectivity of 99.8% based on the reacted methyl 3-carbamoylisobutyrate, and formamide at a selectivity of 98.4% based on the same. The sodium methylate in the reaction liquid was neutralized with sulfuric acid, and subsequently the reaction liquid was distilled by a conventional method. As a result, methyl formate and methanol were recovered and there were obtained 60 g of dimethyl methylsuccinate with at least 99% purity and 16 g of formamide with 99% purity. The recovery of these substances inclusive of an intermediate fraction was quantitative, respectively.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05618953uspto-grants-1997_04