반응 #81643

ord-e5055da4b54a4b05b2c5db3de2eb6879

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도with heating
  2. 2
    온도to maintain the internal pressure at 40 kg/cm2G
  3. 3
    기타reached 60° C.
  4. 4
    온도to maintain the internal pressure at 40 kg/cm2G
  5. 5
    기타to proceed with the reaction for 3 hours
  6. 6
    온도Subsequently, the content therein was cooled
  7. 7
    기타As a result of analysis

실험 절차

The procedure in Example 3 (3) was repeated to proceed with heating stirring reaction except that in place of 180 g of methyl formate and 96 g of methanol, 200 g of methanol was charged in the autoclave and carbon monoxide was pressurized into the autoclave so as to maintain the internal pressure at 40 kg/cm2G. After the temperature of the content in the autoclave reached 60° C., carbon monoxide was fed in the autoclave so as to maintain the internal pressure at 40 kg/cm2G to proceed with the reaction for 3 hours. Subsequently, the content therein was cooled, internal pressure was gradually lowered to atmospheric pressure, and the reaction product was taken out. As a result of analysis therefor, the conversion of methyl 3-carbamoylisobutyrate was 81.4% and there were obtained dimethyl methylsuccinate at a selectivity of 95.7% and formamide at a selectivity of 94.4%, each based on the reacted methyl 3-carbamoylisobutyrate.

출처

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