HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,1'-Carbonyldiimidazole → 1H-Imidazole-1-carboxamide, N-(2,2-dimethoxyethyl)-
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| Reactant | Aminoacetaldehyde dimethyl acetal | HCID 89728 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 1H-Imidazole-1-carboxamide, N-(2,2-dimethoxyethyl)- | HCID 18763368 | 70% |
Reaction Steps
A mixture of 1,1′-carbonylbis[1H-imidazole] (2 mol) in EtOAc (800 ml) was stirred and cooled on an ice-bath, resulting in a suspension. 2,2-dimethoxyethanamine (2 mol) was added dropwise while the temperature was kept below 25 ° C. The resulting reaction mixture was stirred for 2 hours at RT, then for 30 minutes while cooling on an ice-bath. The precipitate was filtered off, stirred in EtOAc (400 ml) during 15 minutes, and on an ice-bath during 15 minutes. The precipitate was filtered off, washed with DIPE (2×50 ml), and dried, yielding 277 g (70%) of N-(2,2-dimethoxyethyl)-1H-imidazole-1-carboxamide (interm. 5).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06656959B1 |
| Source dataset | uspto-grants-2003_12 |
| ORD ID | ord-28392dbf7be24a88957b82801723f1a0 |
| Source note | uspto-grants-2003_12 |