Water → 2-Bromo-6-iodo-3-methoxypyridine

HRID 506769

Reaktionsgleichung

[CH3:1]I.[Br:3][C:4]1[C:9]([OH:10])=[CH:8][CH:7]=[C:6]([I:11])[N:5]=1.O>CN(C=O)C>[Br:3][C:4]1[C:9]([O:10][CH3:1])=[CH:8][CH:7]=[C:6]([I:11])[N:5]=1

Komponenten

Reaktionsbedingungen

Temperatur: 100 °C

Versuchsvorschrift

Add K2CO2 (6.22 g, 45.1 mmol) and methyl iodide (24.6 g, 10.77 mL, 173.3 mmol) to 2-bromo-6-iodopyridin-3-ol, 2 (14.9 g, 49.5 mmol), dissolved in DMF (30 mL). Heat the reaction medium at 100° C. for 2 h, then leave it to cool to room temperature. Then stop the reaction with H2O and stir it for a further 30 min. The precipitate is then filtered, washed with H2O and dried in air to give 3 (15.7 g, 100%) in solid form, light brown: 1H NMR (CDCl3) δ 7.61 (d, 1H, J=8.4 Hz), 6.86 (d, 1H, J=8.4 Hz), 3.93 (s, 3H); m/z obs.=314 (M+1), 315.

Aufarbeitung

customleave it
temperatureto cool to room temperature
filtrationThe precipitate is then filtered
washwashed with H2O
customdried in air

Quellen und Nachweise

ORD-Eintrag: ord-ac1f9cc4e7ae4f0d859fadbd384831a8
Quelldatensatz: uspto-grants-2010_08
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US07786114B2

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