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HRID 17342Erstellt: 25. Oktober 2026

Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) → HCID 68585884, Verbindung

https://huagongshe.com/reaction/17342

Reaktionsgleichung

Beteiligte Stoffe

RolleNameHCIDEinwaage
EduktBenzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1)HCID 466102—
EduktN-(4-Acetyl-2-cyano-5-fluoro-6-hydroxy-3-methylphenyl)cyclopropanecarboxamideHCID 86630836—
LösungsmittelTolueneHCID 1140—
LösungsmittelEthyl AcetateHCID 8857—
ProduktHCID 68585884HCID 6858588471,5%

Reaktionsschritte

N-(4-Acetyl-2-cyano-5-fluoro-6-hydroxy-3-methylphenyl)cyclopropanecarboxamide (I-81) (200 mg, 0.72 mmol) was dissolved in toluene (4 ml), pyridinium p-toluenesulfonate (40 mg, 0.14 mmol) was, added, followed by heating under reflux for 21 hours. After cooling to room temperature, this was diluted with ethyl acetate, washed with water and saturated brine. The obtained organic layer was dried over anhydrous sodium sulfate, the solvent was evaporated away under reduced pressure. The resulting residue was subjected to silica gel column chromatography, eluted with a mixed solvent of n-hexane/ethyl acetate (3:1, v/V) to obtain the entitled compound (133 mg, 71%) as a white solid.

Herkunft & Nachweise

DOI10.6084/m9.figshare.5104873.v1
PatentnummerUS07737166B2
Quelldatensatzuspto-grants-2010_06
ORD IDord-f2b23d306e474821bdd0557cf0e49d6d
Quellennotizuspto-grants-2010_06