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Process for producing 2-methyl-8-nitryl quinoline

A technology of nitroquinoline and methyl, which is applied in the preparation of 2-methyl-8-nitroquinoline and the synthesis process of chemical raw materials, which can solve the problems of high harm to the human body and the environment, low yield, and process pollution etc. to achieve low cost, high yield and high product purity

Inactive Publication Date: 2009-05-13
CINIC CHEM SHANGHAI
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Problems solved by technology

[0003] The object of the present invention is to provide a kind of preparation method of 2-methyl-8-nitroquinoline, the preparation method of described this 2-methyl-8-nitroquinoline will solve the preparation in the prior art The process of 2-methyl-8-nitroquinoline is seriously polluted, very harmful to the human body and the environment, and the technical problem of low yield

Method used

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Embodiment Construction

[0017] Put 1450Kg concentrated hydrochloric acid, 500Kg o-nitroaniline and 4000Kg benzene solvent into the reaction kettle, stir to form a uniform dispersion, keep it for 1 hour, at the set temperature, add 500Kg of paraldehyde dropwise, keep the temperature for 2 hours, and then Add 46Kg of iodine, continue the insulation reaction for 2 hours, cool to about 40°C, separate the hydrochloride solution of 2-methyl-8-nitroquinoline,

[0018] Add 5000Kg water to the hydrochloride solution of 2-methyl-8-nitroquinoline, add NH 4 OH solution to PH=9, then separate 2-methyl-8-nitroquinoline,

[0019] Add it into 5000Kg of water, wash with water, filter, and dry in vacuum to obtain 573Kg of 2-methyl-8-nitroquinoline. The GC purity of the product is 95%, and the yield is 80%.

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Abstract

The invention provides a method for preparing 2-methyl-8-nitroquinoline. The method comprises the following steps: o-nitroaniline reacts in hydrochloric acid and benzene solution to form hydrochloride of the o-nitroaniline; the o-nitroaniline hydrochloride and aldehyde are subjected to cyclization at a temperature between 10 and 100 DEG C; oxidation reaction is performed by use of oxidant at a temperature between 10 and 100 DEG C; and finally the 2-methyl-8-nitroquinoline with high purity is obtained through separation, neutralization, washing and drying. The method has the advantages that the method uses low-toxicity paraldehyde as a raw material to replace virulent crotonaldehyde, and uses iodine as the oxidant to replace virulent arsenic acid so as to reduce toxic effects on human and environment; inorganic acid and inorganic base used in the reaction are common acid and base; and the method is low in cost, little in pollution and high in product purity, and reaches the yield of 80 percent.

Description

technical field [0001] The invention belongs to the field of organic chemistry, in particular to a synthesis process of chemical raw materials, in particular to a preparation method of 2-methyl-8-nitroquinoline. Background technique [0002] 2-methyl-8-nitroquinoline is an intermediate used to prepare an organic pigment intermediate 2-methyl-8-aminoquinoline. The prior art uses crotonaldehyde as a raw material and arsenic acid as an oxidant. The disadvantage of the process is that both crotonaldehyde and arsenic acid are highly toxic substances, which are very harmful to the human body and the environment, and the yield is low, only 62%. Contents of the invention [0003] The object of the present invention is to provide a kind of preparation method of 2-methyl-8-nitroquinoline, the preparation method of described this 2-methyl-8-nitroquinoline will solve the preparation in the prior art The technical process of 2-methyl-8-nitroquinoline is seriously polluted, very harmfu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D215/18
Inventor 申兴李秀娟
Owner CINIC CHEM SHANGHAI
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