4-IODO-6-METHOXYPYRIDIN-3-OL synthesis
- Product Name:4-IODO-6-METHOXYPYRIDIN-3-OL
- CAS Number:431942-27-7
- Molecular formula:C6H6INO2
- Molecular Weight:251.02
431942-26-6
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431942-27-7
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Yield:431942-27-7 970 mg
Reaction Conditions:
with hydrogenchloride in tetrahydrofuran;water at 60; for 3 h;
Steps:
3 Step 3. Synthesis of 3-hydroxy-4-iodo-6-methoxypyridine (53)
Intermediate 52 (1400 mg, 4.74 mmol) was dissolved in 7 mL of anhydrous THF at room temperature, and then 10 mL of 3N HCl was added. The reaction was stirred at 60° C. for 3 hours, and then warmed to room temperature overnight. The reaction should be diluted with ethyl acetate (50mL) and (50ml) water, separated into layers, the aqueous phase has more solids, add NaHCO3 to the aqueous phase to pH=4, extract with ethyl acetate (50mL X3), combine the organic phases Wash with 100mL saturated brine, dry with anhydrous sodium sulfate, filter and spin dry to obtain a crude product, which is purified by column chromatography (biotage, 120g, C-18, UV214, acetonitrile in water containing 0.05% TFA 5-95%) ) To obtain Intermediate 53, white solid, 970mg, two-step yield 76%, purity 82%
References:
CN112028877,2020,A Location in patent:Paragraph 0294-0296
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