Back
HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 650498Generated: October 29, 2026

Toluene → HCID 21712145, compound

https://huagongshe.com/reaction/650498

Reaction equation

Participants

RoleNameHCIDCharge
ReactantTolueneHCID 1140—
ReactantLawesson's reagentHCID 87949—
ReactantHCID 21712164HCID 21712164—
SolventDichloromethaneHCID 6344—
ProductHCID 21712145HCID 2171214561.6%

Reaction Conditions

Temperature120 °C

Reaction Steps

0.50 g of 1-benzyl-3-chloro-6-(4-chloro-5-difluoromethoxy-1-methyl-[1H]-pyrazol-3-yl)-5-fluoro-[1H]-pyridin-2-one is introduced into 5 ml of toluene, 0.63 g of Lawesson's reagent is added and the resulting yellow suspension is stirred overnight at 120° C. The next day, the mixture is cooled to 22° C., diluted with methylene chloride and, after the addition of 3 g of silica gel, concentrated to dryness in vacuo. The silica gel is applied to a flash chromatography column and eluted first with toluene/ethyl acetate 30/1 (v/v) and then with n-hexane/ethyl acetate 2/1 (v/v). 0.32 g of the desired title compound is obtained in the form of a yellow solid having a melting point of 135-138° C.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS06274536B1
Source datasetuspto-grants-2001_08
ORD IDord-6e33a53eafe8469d82c7a10cd1049adc
Source noteuspto-grants-2001_08