Synthetic method for irbesartan
A synthesis method and intermediate technology, applied in the field of synthesis of antihypertensive drugs, can solve problems such as complex operation steps, high production cost, and complicated operation, and achieve the effects of simplified operation process, increased yield, and simple process operation
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[0030] The invention will be further described below in conjunction with the examples, and the non-limiting examples are as follows.
[0031] Preparation of intermediate (I) 2-butyl-1,3-diazaspiro[4,4]nonan-1-en-4-one:
[0032] Put 16.5g (0.15mol) of aminocyclopentanitrile in a 250mL flask, add 100mL THF and mechanically stir until the raw material is dissolved, add dropwise a THF solution of 18.0g (0.15mol) of valeryl chloride under stirring, continue stirring for 0.5h, add water 20mL, 50mL of methanol and 20g of potassium hydroxide, reflux for 5h, concentrate under reduced pressure, add water and ethyl acetate to the concentrate for extraction, dry the organic phase with anhydrous magnesium sulfate, filter, and concentrate the filtrate to obtain 27.0g of an oily substance. The rate is 92.7%.
[0033] Intermediate (II) 2-butyl-3-[(2′-cyanobiphenyl-4-yl)methyl]-1,3-diazaspiro[4,4]non-1-ene- Preparation of 4-keto:
[0034] Intermediate (I) 19.4g (0.1mol), 4'-(bromomethyl)-2-...
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