HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 58201184, compound → 3-Chloro-4-methoxy-2,5-dimethylpyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 58201184 | HCID 58201184 | — |
| Catalyst | HCID 178418390 | HCID 178418390 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 3-Chloro-4-methoxy-2,5-dimethylpyridine | HCID 58201214 | 79.7% |
Reaction Steps
The above 3-chloro-5-(chloromethyl)-4-methoxy-2-methylpyridine (550 mg) was dissolved in 10 ml of methanol, and 10% Pd carbon (50 mg) was then added to the solution. Normal-pressure contact hydrogenation was performed on the mixture under cooling on ice for 3 hours. Thereafter, the catalyst was removed by filtration, and methanol was then distilled away under reduced pressure. The residue was extracted with chloroform. The organic layer was washed with a saturated sodium bicarbonate solution, and it was then dried over anhydrous sodium sulfate. The solvent was distilled away, and the residue was purified by silica gel chromatography (ethyl acetate-hexane), so as to obtain the title compound (365 mg) as an oily substance.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08236813B2 |
| Source dataset | uspto-grants-2012_08 |
| ORD ID | ord-f4ca92807c6c4b65aa89817cf88a3d1f |
| Source note | uspto-grants-2012_08 |