HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → 6-Bromo-3-pyridinecarboxaldehyde
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | 2,5-Dibromopyridine | HCID 69353 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | 6-Bromo-3-pyridinecarboxaldehyde | HCID 11769234 | 41% |
Reaction Steps
To a diethyl ether (500 mL) solution of 2,5-dibromopyridine (25 g, 110 mmol) was added dropwise n-butyl lithium (2.67 M n-hexane solution, 45 mL, 120 mmol) at −76° C., which was stirred for 25 minutes. To this solution was added dropwise N,N-dimethylformamide (9.0 mL, 120 mmol) at −76° C. Upon completion of this addition, the reaction solution was gradually cooled to room temperature. This mixture was partitioned into ethyl acetate and water. The organic layer was separated and concentrated under a reduced pressure. The residue was purified by silica gel column chromatography (heptane:ethyl acetate=8:1) to obtain the title compound (8.0 g, 41%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08841327B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-7217fd09e51141518f1e3d19b0b05fe9 |
| Source note | uspto-grants-2014_09 |