HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl propiolate → Methyl 2-methyl-1H-imidazole-5-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl propiolate | HCID 13536 | — |
| Reactant | N-Hydroxyacetamidine | HCID 30926 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | Methyl 2-methyl-1H-imidazole-5-carboxylate | HCID 13432302 | — |
Reaction Steps
A solution of N′-hydroxyethanimidamide (65 g, 880 mmol) in anhydrous methanol (2 L) was treated with methyl propiolate (100 g, 1.19 mol), and the reaction was heated at reflux for 4 hours. The reaction mixture was concentrated in vacuo, and the residue was diluted with diphenyl ether (1 L) and heated at reflux for 4 hours. The hot solution was filtered, and the filtrate was cooled to room temperature and diluted with hexanes (2 L). The resulting solid was washed with diethyl ether (1 L), to afford the product as a brown solid. Yield: 60 g, 430 mmol, 49%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09296761B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-e16061c9c0d340a596addc0648099cde |
| Source note | uspto-grants-2016_03 |