Method for synthesizing 5-iodo-2-pyridineacetic acid
A technique for pyridineacetic acid and its synthesis method, which is applied in the direction of organic chemistry, etc., can solve the problem that 5-iodo-2-pyridineacetic acid cannot be purified and prepared by silica gel chromatography column, and achieves the effect of cheap raw materials and unique reaction circuit
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[0011] step 1:
[0012] Dimethyl sulfoxide (500 mL) was added to a 1-liter three-neck flask, sodium hydride (60%, 27.7 g, 692 mmol) was added at room temperature, tert-butyl cyanoacetate (100.7 g, 713 mmol) was added dropwise, about After dropping for 1 hour, stir at room temperature for half an hour, add 2-bromo-5-iodopyridine (76.7 g, 270 mmol), heat to 125 ° C, react for 6 hours, stop heating, cool to room temperature, stir the reaction solution Slowly pour into the ammonium chloride solution (150 g of ammonium chloride dissolved in 1.5 L of water), the solid precipitated, suction filtered, washed with water, dissolved in about ethyl acetate (2 L), washed with saturated brine, the organic phase Dried, spin-dried, slurried with a mixture of ethyl acetate and petroleum ether (volume ratio 1:10, 200 mL), filtered the solid with suction, transferred it to a paper tray to dry overnight, and obtained a yellow solid, the target compound 1 (54 g, 157 mmol, 58%);
[0013] Step 2: ...
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