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HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
HRID 533527Erstellt: 26. Oktober 2026

Hydrochloric Acid → HCID 86668761, Verbindung

https://huagongshe.com/reaction/533527

Reaktionsgleichung

Beteiligte Stoffe

RolleNameHCIDEinwaage
EduktHydrochloric AcidHCID 313—
EduktLithium HydroxideHCID 3939—
EduktTetrahydrofuran-methanol waterHCID 66577907—
EduktEthyl 4-(6-bromopyridin-3-yl)-2-methyl-2-(methylsulfonyl)butanoateHCID 86668759—
LösungsmittelWaterHCID 962—
ProduktHCID 86668761HCID 86668761101,4%

Reaktionsschritte

A solution of lithium hydroxide (357 mg, 8.5 mmol, 4.0 equiv) and ethyl 4-(6-bromopyridin-3-yl)-2-methyl-2-(methylsulfonyl)butanoate (775 mg, 2.1 mmol, 1.0 equiv) in 1:1:1 tetrahydrofuran-methanol-water (3 mL) was allowed to stir at room temperature for 2 h. The reaction was diluted with water (150 mL), acidified (to pH=2) with 0.5 M hydrochloric acid, and then was extracted with ethyl acetate (3×100 mL). The combined organic layers were washed with brine (100 mL), dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure to provide the title compound (716 mg, 98%). MS (LCMS) m/z 334.1 (M−1). 1H NMR (400 MHz, CHLOROFORM-d) δ ppm 1.56 (s, 3H) 2.03 (td, J=12.78, 5.27 Hz, 1H) 2.31 (td, J=12.68, 4.68 Hz, 1H) 2.51 (td, J=12.98, 4.49 Hz, 1H) 2.59-2.70 (m, 1H) 2.96 (s, 3H) 7.30-7.39 (m, 2H) 8.07 (d, J=1.56 Hz, 1H).

Herkunft & Nachweise

DOI10.6084/m9.figshare.5104873.v1
PatentnummerUS08853258B2
Quelldatensatzuspto-grants-2014_10
ORD IDord-3cf975d366cf4e32b5a686ddc850d8c2
Quellennotizuspto-grants-2014_10