Preparation method of isopropyl 2-(3-nitrobenzylidene)acetoacetate

A technology of isopropyl acetate and nitrobenzylidene, applied in the field of medicine, can solve problems such as increasing the cost of industrialized production, unsatisfactory yield, etc., achieves improved yield and purity, shortened reaction time, and cheap and easy-to-obtain raw materials Effect
CN102491902AInactive Publication Date: 2012-06-13QINGDAO HUANGHAI PHARM CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Current Assignee / Owner
QINGDAO HUANGHAI PHARM CO LTD
Publication Date
2012-06-13
Estimated Expiration
Not applicable · inactive patent

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Abstract

The invention provides a preparation method of isopropyl 2-(3-nitrobenzylidene)acetoacetate, which comprises the following steps: carrying out condensation reaction on 3-nitrobenzaldehyde and isopropyl acetoacetate as initial raw materials by using an organic solvent as a solvent in the presence of catalysts acetic acid and piperidine for 2-8 hours; after carrying out vacuum concentration on the filtrate at 80 DEG C to 2 / 3-3 / 4 by volume, cooling to -5-5 DEG C while stirring to crystallize over night; and filtering, and recrystallizing with isopropanol to finally obtain the isopropyl 2-(3-nitrobenzylidene)acetoacetate. The invention shortens the reaction time; the isopropanol, which has lower toxicity than methylbenzene and can enhance the product yield and purity, is utilized as the reaction solvent; the catalytic rate of the catalysts is very high, the reaction is quicker and more thorough, and thus, the catalysts can enhance the yield; the invention enhances the yield and saves the cost; and since the refinement method of column chromatography separation, the technique is easy to operate, has the advantage of cheap and accessible raw materials, and thus, is suitable for industrial production.
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Description

technical field

[0001] The invention belongs to the field of medicine, in particular to a preparation method of 2-(3-nitrobenzylidene) isopropyl acetoacetate. Background technique

[0002] Azclnidipine (Azclnidipine) is a new type of dihydropyridine drug, which was jointly developed by Sankyo and Ube Industries in Japan. Calcium channel blockers for blood pressure are currently on the market in more than a dozen countries around the world. It is a promising antihypertensive drug, and its effect is more specific. It is widely used clinically to lower blood pressure in mild or moderate essential hypertension, renal disorder with hypertension, and severe hypertension. Very good market prospects.

[0003] 2-(3-nitrobenzylidene) isopropyl acetoacetate is one of the key intermediates in the synthesis of azedipine. At present, there are many reports about the preparation method of 2-(3-nitrobenzylidene) isopropyl acetoacetate. Society, 1982. ) After dissolving m-nitrobenzaldehy...

Claims

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