HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 15979330, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | HCID 69297227 | HCID 69297227 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Sodium Hydroxide | HCID 14798 | — |
| Product | HCID 15979330 | HCID 15979330 | 43% |
Reaction Steps
In a 25 ml, three-necked flask fitted with a magnetic stirrer, a reflux condenser and a dropping funnel under inert atmosphere, 150 mg (0.61 mmol) of 1-methyl-5-[(2-oxo-4-propylpyrrolidin-1-yl)methyl]-1H-imidazole-4-carbonitrile 122 is dissolved in MeOH (9 ml) with water (3 ml) and aqueous NaOH (35% w/w, 30 μl). The reaction mixture is refluxed 72 h, cooled down to room temperature and the solvent is evaporated to dryness. The crude reaction mixture is purified by preparative chromatography on silicagel (CH2Cl2/MeOH/NH4OH: 96/3.6/0.4 (v/v/v/v)) and recristallized in CH2Cl2/hexane to afford 1-methyl-5-[(2-oxo-4-propylpyrrolidin-1-yl)methyl]-1H-imidazole-4-carboxamide 123 (0.07 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08178533B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-0dc5d6ec8b8143cfac9257ce039effce |
| Source note | uspto-grants-2012_05 |