HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → HCID 68158303, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 68158987 | HCID 68158987 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Sulfuric Acid | HCID 1118 | — |
| Product | HCID 68158303 | HCID 68158303 | 84% |
Reaction Steps
A solution of 5-(bromomethyl)-1-methyl-4-nitro-1H-imidazole-2-carbonitrile (264) (70 mg, 0.29 mmol) in 90% H2SO4 (1 mL) was heated at 65-70° C. for 1 hour, before being diluted with water and given a standard ethyl acetate workup to give 5-(bromomethyl)-1-methyl-4-nitro-1H-imidazole-2-carboxamide (266) (67 mg, 84%), as white solid, m.p. 220-222° C. 1H NMR [(CD3)2SO] δ 8.18 (s, 1H), 7.87 (s, 1H), 5.05 (s, 2H), 4.02 (s, 3H). HR-MS (APC+, 79/81Br) found: m/z 262.9770/264.9752 (M+1), calcd. for C6H879/81BrN4O3+: 262.9774/264.9754.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09101632B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-e33b66e854ae46529c8f7deff2ed7219 |
| Source note | uspto-grants-2015_08 |