HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → Ethyl 3-{[(4,5-dimethyl-1H-benzimidazol-2-yl)methyl]amino}-1H-pyrrole-2-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Ethyl 3-amino-1H-pyrrole-2-carboxylate | HCID 2773439 | — |
| Reactant | Sodium cyanoborohydride | HCID 5003444 | — |
| Reactant | 4,5-Dimethyl-1H-benzo[d]imidazole-2-carbaldehyde | HCID 45120761 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | Ethyl 3-{[(4,5-dimethyl-1H-benzimidazol-2-yl)methyl]amino}-1H-pyrrole-2-carboxylate | HCID 67068491 | 27.5% |
Reaction Steps
3-Amino-1H-pyrrole-2-carboxylic acid ethyl ester (0.077 g, 0.5 mmol), 4,5-dimethyl-1H-benzimidazole-2-carbaldehyde (0.130 g, 0.75 mmol) and HOAc (0.045 g, 0.75 mmol) were stirred in methanol (4 mL) followed by addition of NaCNBH3. The resulting mixture was stirred at r.t. for 16 h. The reaction mixture was neutralized with 2M NaOH and the solvent was removed in vacuo. The residue was dissolved in ethyl acetate and extracted with water. The organic layer was dried (Na2SO4) and concentrated. The crude product was purified by flash column chromatography (heptane/ethyl acetate gradient; 0 to 100% ethyl acetate), obtaining a white solid, 0.043 g (27%) of the title compound, as a tautomeric mixture (1:1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07829707B2 |
| Source dataset | uspto-grants-2010_11 |
| ORD ID | ord-1b6e509cf8be414480804c56d951eeac |
| Source note | uspto-grants-2010_11 |