HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → 4-(4-Bromo-pyridin-2-yl)-4-oxo-butyraldehyde
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 58191758 | HCID 58191758 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 4-(4-Bromo-pyridin-2-yl)-4-oxo-butyraldehyde | HCID 58191780 | — |
Reaction Steps
To a solution of 1-(4-bromo-pyridin-2-yl)-4,4-dimethoxy-butan-1-one (2) (crude from Step 2, 11 g, 38.2 mmol) in 100 of CH2Cl2 at room temperature is added trifluoroacetic acid (10.9 g, 95.4 mmol) and the reaction mixture is stirred overnight. The reaction is concentrated, the residue dissolved in ethyl acetate (150 mL) and washed with water 3 times. The organic layers are combined, dried over Na2SO4 and the solvent evaporated. The residue is purified by flash column chromatography (30% EtOAc in hexanes) to give 4-(4-bromo-pyridin-2-yl)-4-oxo-butyraldehyde (3) as an yellow oil. (4.16 g, 45%): MS ES+244.04.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08546336B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-4a2695e74ca14d3bbbf8006355b6c42e |
| Source note | uspto-grants-2013_10 |