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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 877023Generated: October 31, 2026

HCID 2778795, compound → HCID 178474418, compound

https://huagongshe.com/reaction/877023

Reaction equation

Participants

RoleNameHCIDCharge
ReactantHCID 2778795HCID 2778795—
ReactantHCID 178475102HCID 178475102—
SolventWaterHCID 962—
SolventAcetonitrileHCID 6342—
SolventEthyl AcetateHCID 8857—
ProductHCID 178474418HCID 17847441825.5%

Reaction Steps

To a stirred solution of 2-bromo-1-[3-fluoro-4-(trifluoromethyl)phenyl]ethanone (4.5 g, 15.73 mmol) in acetonitrile (45 ml) was added acetyl guanidine (2.38 g, 23.60 mmol) at room temperature. After refluxing for 4 h the reaction mixture was cooled to room temperature and diluted with ethyl acetate and water. The layers were separated. The aqueous layer was extracted 2-3 times with ethyl acetate and the combined organic layers were washed with water, followed by brine, dried (Na2SO4) and filtered. The filtrate was concentrated under reduced pressure. The residue obtained after the evaporation of the solvent was purified by silica gel column chromatography using 2% methanol in chloroform to obtain 1.15 g of the product as a yellow solid; 1H NMR (300 MHz, DMSO-d6) δ 2.07 (s, 3H), 7.58 (s, 1H), 7.69-7.78 (m, 3H), 11.31 (br s, 1H), 11.91 (br s, 1H).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08987278B2
Source datasetuspto-grants-2015_03
ORD IDord-455892e829b24b1b925babe90a1c9c73
Source noteuspto-grants-2015_03