HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 877023Generated: October 31, 2026
HCID 2778795, compound → HCID 178474418, compound
https://huagongshe.com/reaction/877023
Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | HCID 2778795 | HCID 2778795 | — |
| Reactant | HCID 178475102 | HCID 178475102 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 178474418 | HCID 178474418 | 25.5% |
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
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08987278B2 |
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| Source dataset | uspto-grants-2015_03 |
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| ORD ID | ord-455892e829b24b1b925babe90a1c9c73 |
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| Source note | uspto-grants-2015_03 |
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