1-(2-FLUORO-4-IODO-3-PYRIDINYL)-ETHANONE synthesis
- Product Name:1-(2-FLUORO-4-IODO-3-PYRIDINYL)-ETHANONE
- CAS Number:1160502-25-9
- Molecular formula:C7H5FINO
- Molecular Weight:265.02
744257-63-4
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1160502-25-9
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Yield:1160502-25-9 60%
Reaction Conditions:
with manganese(IV) oxide in toluene; for 1.58333 h;Heating / reflux;
Steps:
10.B
l-(2-fluoro-4-iodopyridin-3-yl)ethanol (3.25 g, 12.17 mmol) was dissolved in dry Toluene (40 mL) and MnO2 (12.45 g, 121.7 mmol) was added in one portion. The resultant suspension was stirred at reflux for 95 minutes. Reaction mixture allowed to cool to RT and filtered through celite, washing copiously with EtOAc. The filtrate was concentrated under reduced pressure to give an orange/brown oil. This material was redissolved in DCM and vacced down onto silica (~30mL). The resulting solid was purified by column chromatography (15% EtOAc in hexanes, ~300mL silica) to give a light yellow oil, which solidified on cooling in an ice-bath to give a light yellow solid (1.92g, 60% Yield). IH NMR (400.0 MHz, DMSO: 2.57 (3H, s), 7.95 (IH, d), 8.03 (IH, d).
References:
WO2009/73300,2009,A1 Location in patent:Page/Page column 147
113975-22-7
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1160502-25-9
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