Preparation method of muscarinic receptor antagonist glycopyrronium bromide
A technology of muscarinic receptors and glycopyrronium bromide, applied in the field of medicine
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[0013] Alpha-cyclopentylmandelic acid (5)
[0014] Magnesium chips (1.5g, 62mmol), anhydrous ether (20mL) and a small amount of iodine were added to a 250mL three-necked flask. Heated to 30°C, and a small amount of bromocyclopentane ( 3 ) diethyl ether solution, heating to initiate the reaction, when the iodine color disappears, add dropwise under stirring 3 (8.94g, 60mmol) in diethyl ether (15mL), heated to 37°C and refluxed for 20min after dropping, then cooled to 0~5°C. Join in batches 2 (3g, 20mmol), after the addition, add 40mL of anhydrous diethyl ether, raise the temperature to 30°C, stir for 10h, add hydrochloric acid (30mL, 4 mol / L) and stir until the solid is completely dissolved, separate the diethyl ether layer, and wash the water layer with diethyl ether (20mL , 20mL, 10mL) extracted three times. Combine the ether layers, extract twice with 10% sodium carbonate aqueous solution (60mL, 40mL), combine the water layers, adjust the pH to 1~2 with concentrated hy...
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