Reaktion #960243

Reaktionsgleichung

hydrogen peroxide water

2,3-difluoro-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine

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title product

Ausbeute 29.6%

5,6-difluoropyridin-3-ol

Ausbeute 29.6%

Lösungsmittel

water

tetrahydrofuran

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionextracted with ethyl acetate
2. 2
   WaschenCombined organic portions were washed with aqueous 5% sodium thiosulfate solution and saturated saline water
3. 3
   Trocknendried over anhydrous sodium sulfate
4. 4
   Einengenconcentrated
5. 5
   SonstigePurification via Biotage Spla HPFC system (C18, mobile phase: 0.01% NH4HCO3, CH3CN/water, 10˜95%)

Vorschrift

A mixture of hydrogen peroxide water (1.50 mL, 13.2 mmol) and 2,3-difluoro-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine (2.8 g) in tetrahydrofuran (15 mL) was stirred at room temperature for 2 h, then diluted with water and extracted with ethyl acetate. Combined organic portions were washed with aqueous 5% sodium thiosulfate solution and saturated saline water, dried over anhydrous sodium sulfate and concentrated. Purification via Biotage Spla HPFC system (C18, mobile phase: 0.01% NH4HCO3, CH3CN/water, 10˜95%) afforded the title product as a white solid (450 mg).

Quelle