HuagongsheHuagongshe Chemistry Print Report · For research reference only
Carbamic acid, ethyl ester → HCID 13765531, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Carbamic acid, ethyl ester | HCID 5641 | — |
| Reactant | Methacrolein | HCID 6562 | — |
| Catalyst | 4-Methoxyphenol | HCID 9015 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 13765531 | HCID 13765531 | 60.8% |
Reaction Steps
35 g of methacrolein are added dropwise at 60°-65° C. to a mixture of 133.5 g of ethyl carbamate, 30 g of acid ion exchanger resin (Duolite C 265), 0.4 g of hydroquinone monomethyl ether and 400 ml of chloroform in the course of 40 minutes. The mixture is left at that temperature for 1 hour, the ion exchanger is filtered off, the chloroform is distilled off, and the residue is crystallized from ethyl acetate/petroleum ether. This gives 97 g of 2-methyl-1,1,3-tri(ethoxycarbonylamino)propane (60.8% yield, based on starting methacrolein) having a melting point of 138°-140° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04672137 |
| Source dataset | uspto-grants-1987_06 |
| ORD ID | ord-c525e6be7e7b49e8ad067f8a2b7db111 |
| Source note | uspto-grants-1987_06 |