HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methane → HCID 86741873, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methane | HCID 297 | — |
| Reactant | L-Methionine | HCID 6137 | — |
| Reactant | Diphosgene | HCID 10426 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 86741873 | HCID 86741873 | — |
Reaction Steps
0.35 mol diphosgene is added dropwise over 1 hour to a mixture of 0.28 mol of the methyl ester of methionine and 0.4 g activated charcoal in 400 mL dioxane under N2. The reaction mixture is then heated and stirred at reflux for 21/2 hours. The reaction mixture is then cooled, filtered, and concentrated to dryness by rotary evaporator, keeping exposure to moisture to a minimum. The crude product is re-dissolved in 100 mL THF, and the pH of the solution is adjusted to 5.5-6.0 by addition of pyridine. The product mixture is again filtered, and the filtrate is fractionally distilled to give methionine methyl ester isocyanate.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04705864 |
| Source dataset | uspto-grants-1987_11 |
| ORD ID | ord-bd4e2d89716b402d9576529c7c4bdaa5 |
| Source note | uspto-grants-1987_11 |