Réaction #81643

ord-e5055da4b54a4b05b2c5db3de2eb6879

Équation de réaction

[C]=O
carbon monoxide
COC(=O)C(C)CC(N)=O
methyl 3-carbamoylisobutyrate
COC=O
methyl formate
[C]=O
carbon monoxide
COC(=O)CC(C)C(=O)OC
dimethyl methylsuccinate
NC=O
formamide

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Températurewith heating
  2. 2
    Températureto maintain the internal pressure at 40 kg/cm2G
  3. 3
    Autrereached 60° C.
  4. 4
    Températureto maintain the internal pressure at 40 kg/cm2G
  5. 5
    Autreto proceed with the reaction for 3 hours
  6. 6
    TempératureSubsequently, the content therein was cooled
  7. 7
    AutreAs a result of analysis

Mode opératoire

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.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US05618953uspto-grants-1997_04