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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 128859Generated: November 1, 2026

Benzene → HCID 18688800, compound

https://huagongshe.com/reaction/128859

Reaction equation

Participants

RoleNameHCIDCharge
ReactantBenzeneHCID 241—
ReactantTriethylamineHCID 8471—
Reactant2,4-DifluoroanilineHCID 9709—
ReactantP,P-Diphenylphosphinic azideHCID 199401—
ReactantHCID 18688868HCID 18688868—
SolventWaterHCID 962—
ProductHCID 18688800HCID 1868880055.8%

Reaction Steps

To a stirred mixture of 1.05 g of 1-(p-toluenesulfonyl)-3-phenylindole-3-carboxylic acid and 0.60 cc of diphenylphosphoryl azide in 10 cc of benzene was added dropwise 0.39 cc of triethylamine at room temperature. The resulting mixture was stirred at room temperature for 15 minutes and then heated under reflux for 30 minutes. After cooling, 0.285 cc of 2,4-difluoroaniline was added and then stirred at room temperature for 30 minutes, followed by refluxing for 2 hours. After cooling, water was added to the reaction mixture and extracted with ethyl acetate. The extract was dried over magnesium sulfate, and distilled to remove the solvent. The crude product thus obtained was purified by a silica gel column chromatography (eluent: ethyl acetate/hexane=1/3) to obtain 780 mg of compound 120. Yield 55.8%, m.p. 244°-246° C.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS05464863
Source datasetuspto-grants-1995_11
ORD IDord-79fe91e70b97438e98aab6a9e21c202d
Source noteuspto-grants-1995_11