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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1829732Generated: November 3, 2026

Sodium Sulfide → HCID 501227, compound

https://huagongshe.com/reaction/1829732

Reaction equation

Participants

RoleNameHCIDCharge
ReactantSodium SulfideHCID 14804—
ReactantBenzene, 2-(chloromethyl)-1,4-dimethyl-HCID 69987—
Reactant2,3-Dichloro-1-oxo-1lambda~5~-pyridineHCID 21785300—
SolventWaterHCID 962—
ProductHCID 501227HCID 501227—

Reaction Conditions

Temperature70 °C

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

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS07064139B2
Source datasetuspto-grants-2006_06
ORD IDord-283e317c71304008a86cce2dd12b3305
Source noteuspto-grants-2006_06