Reaktion #81641
ord-f419fd2893ef45fb8f0259106ff5352c
Reaktionsgleichung
Reagenzien
Reaktionsbedingungen
Aufarbeitung
- 1Sonstigesubsequently the reaction liquid
- 2workup.DISTILLATIONwas distilled by a conventional method
- 3SonstigeAs a result, methyl formate and methanol were recovered
Vorschrift
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.