HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 4-[2-(3-bromophenyl)-2-oxo-acetyl]-1H-pyrrole-2-carbonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| Reactant | Potassium Permanganate | HCID 516875 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 4-(3-bromo-phenylethynyl)-1H-pyrrole-2-carbonitrile | HCID 68699371 | — |
| Solvent | Acetone | HCID 180 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | Ethyl acetate hexane | HCID 21226206 | — |
| Product | 4-[2-(3-bromophenyl)-2-oxo-acetyl]-1H-pyrrole-2-carbonitrile | HCID 58792270 | 84% |
Reaction Steps
A solution of 4-(3-bromo-phenylethynyl)-1H-pyrrole-2-carbonitrile (2.85 g, 10.52 mmol) in acetone was treated with a 45° C. solution of magnesium sulfate (1.90 g, 15.78 mmol) and sodium bicarbonate (0.53 g, 6.31 mmol) in water, immediately treated with KMnO4 (3.74 g, 23.67 mmol), stirred for 15 minutes (TLC (silica gel, 25% ethyl acetate/hexane) indicated complete clean conversion), diluted with EtOAc and washed with water until the washings were colorless. The organic phase was dried (MgSO4), filtered and evaporated. The resultant residue was crystallized to purity from warm ethyl acetate/hexane to afford 4-[2-(3-bromophenyl)-2-oxo-acetyl]-1H-pyrrole-2-carbonitrile as a yellow crystalline solid, 2.68 g, 84% yield.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07705030B2 |
| Source dataset | uspto-grants-2010_04 |
| ORD ID | ord-e55ded96fe654b1892f5d05c1823adfc |
| Source note | uspto-grants-2010_04 |