Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Sulfide | HCID 14804 | — |
| Reactant | Benzene, 2-(chloromethyl)-1,4-dimethyl- | HCID 69987 | — |
| Reactant | 2,3-Dichloro-1-oxo-1lambda~5~-pyridine | HCID 21785300 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 501227 | HCID 501227 | — |
Reaction Steps
2,3-Dichloropyridine N-oxide (4.3 g, 0.026 mole) (prepared according to U.S. Pat. No. 3,850,939) and sodium sulfide (3.4 g, 0.026 mole) were mixed with 25 mL of water then heated to 70° C. for two hours. The resulting mixture was cooled to room temperature and treated with 2,5-dimethylbenzyl chloride (4.3 g, 0.026 mole) drop wise. After the addition, the mixture was heated to 70° C. for four hours, then cooled in an ice bath. The precipitated solid was filtered and washed with cold toluene leaving 3.5 g of product. Recrystallization from toluene afforded pure product of m.p. 77–80° C. The compound was identified by its NMR spectrum.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07064139B2 |
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| Source dataset | uspto-grants-2006_06 |
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| ORD ID | ord-283e317c71304008a86cce2dd12b3305 |
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| Source note | uspto-grants-2006_06 |
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