HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 58201192, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Sodium Methoxide | HCID 10942334 | — |
| Reactant | Methyl 4,5-dichloro-6-methyl-3-pyridinecarboxylate | HCID 58201215 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 58201192 | HCID 58201192 | 56.4% |
Reaction Steps
Crude methyl 4,5-dichloro-6-methylnicotinate (380 mg) was dissolved in 3 ml of methanol and, in a nitrogen stream, sodium methoxide (120 mg) was then added to the solution under cooling on ice. The temperature of the reaction solution was gradually raised to room temperature, and it was stirred for 18 hours. After the disappearance of the materials had been confirmed, a saturated ammonium chloride aqueous solution was added to the reaction solution under cooling on ice, followed by extraction with chloroform. The organic layer was dried over anhydrous sodium sulfate, and the solvent was then distilled away. The residue was purified by silica gel chromatography (ethyl acetate-hexane), so as to obtain the title compound (210 mg) as a solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08846703B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-6703fede0bb64b7b9bf02fffe8cff39b |
| Source note | uspto-grants-2014_09 |