반응식
[C:1]([CH2:4][CH:5]([CH3:10])[C:6]([O:8][CH3:9])=[O:7])(=[O:3])[NH2:2].[CH:11](N)=[O:12].C[O-].[Na+].S(=O)(=O)(O)O>>[CH3:10][CH:5]([CH2:4][C:1]([O:12][CH3:11])=[O:3])[C:6]([O:8][CH3:9])=[O:7].[CH:1]([NH2:2])=[O:3]참가 물질
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.
후처리
- customsubsequently the reaction liquid
- distillationwas distilled by a conventional method
- customAs a result, methyl formate and methanol were recovered
출처 및 근거
- ORD 기록
- ord-f419fd2893ef45fb8f0259106ff5352c
- 출처 데이터셋
- uspto-grants-1997_04
- 특허 번호
- US05618953
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