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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1039990Generated: October 30, 2026

p-Toluenesulfonic acid → HCID 67256257, compound

https://huagongshe.com/reaction/1039990

Reaction equation

Participants

RoleNameHCIDCharge
Reactantp-Toluenesulfonic acidHCID 6101—
Reactant1,4-DioxaneHCID 31275—
Reactant2-Chloro-4-(trifluoromethyl)pyrimidineHCID 2773912—
Reactant3-Bromo-4-fluoroanilineHCID 2779286—
SolventEthyl AcetateHCID 8857—
ProductHCID 67256257HCID 6725625789.3%

Reaction Steps

To 3-bromo-4-fluoroaniline (0.76 g, 4.0 mmol) and 2-chloro-4-(trifluoromethyl)pyrimidine (0.73 g, 4.0 mmol) was added dioxane (13.33 mL) and p-TSA (0.761 g, 4.0 mmol). The reaction was sealed and was heated at reflux overnight. The reaction was cooled to room temperature and was diluted with ethyl acetate, washed with saturated aqueous NaHCO3, and the organic was dried over sodium sulfate and filtered before concentration. The crude product was purified by flash chromatography (25:75 ethyl acetate:hexanes) to afford N-(3-bromo-4-fluorophenyl)-4-(trifluoromethyl)pyrimidin-2-amine (1.2 g, 3.57 mmol, 89%) as a pale yellowish solid. 1H NMR (500 MHz, CDCl3): δ 8.68 (d, J=4.9 Hz, 1H); 7.99-7.96 (m, 1H); 7.51 (d, J=8.4 Hz, 1H); 7.29 (s, 1H); 7.14 (t, J=8.5 Hz, 1H); 7.10 (d, J=4.9 Hz, 1H). rhSYK activity=+

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08551984B2
Source datasetuspto-grants-2013_10
ORD IDord-346682386d324493a54da1e8e54d8695
Source noteuspto-grants-2013_10