3-iodine-5-methoxypyridine synthesis method
A technology of methoxypyridine and synthesis method, which is applied in the field of synthesis of 3-iodo-5-methoxypyridine, and achieves the effect of simple reaction conditions and easy separation
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Embodiment 1
[0010] step 1:
[0011] Add 3-amino-5-methoxypyridine (10.0 g, 80.6 mmol) and 1.6 M sulfuric acid solution (200 mL) into the three-necked flask; add sodium nitrite (6.0 g, 88.6 mmol) at -5°C. The reaction solution was stirred at -5°C for 10 minutes. Add potassium iodide (40.0 g, 242 mmol) aqueous solution (100 mL) at -5°C and stir at -5°C for 15 minutes. The reaction solution was basified with 2 M sodium hydroxide solution until the pH was equal to 8-9, water (100 mL) was added, extracted with ethyl acetate (100 mL x 3); the organic phases were combined, and saturated sodium bisulfite solution (100 mL) and saturated brine (100 mL), dried over sodium sulfate, and filtered. The filtrate was spin-dried, and the crude product was separated by silica gel column chromatography (petroleum ether: ethyl acetate volume ratio = 40:1) to obtain a white solid, the target compound 1 (10.2 g, 43.4 mmol, 48 %). 1 H NMR (300 MHz, D 2 O) 8.38 (d, J = 2.7 Hz, 1H), 8.28(d, J = 2.7 Hz, 1H), 7....
Embodiment 2
[0012] Example 2, step 1: the reaction time of 3-amino-5-methoxypyridine and sodium nitrite in 1.6 M sulfuric acid solution is 5 minutes, and the reaction temperature is 0 ° C; the reaction time of diazonium salt and potassium iodide is 10 minutes, Reaction temperature is 0 ℃, all the other are with embodiment 1.
Embodiment 3
[0013] Example 3, Step 1: The reaction time of 3-amino-5-methoxypyridine and sodium nitrite in 1.6 M sulfuric acid solution is 15 minutes, and the reaction temperature is -10°C; the reaction time of diazonium salt and potassium iodide is 20 minutes , the reaction temperature is-10°C, and the rest are the same as in Example 1.
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