Synthetic method of high-yield o-hydoxybenzonitrile

A synthesis method, salicylonitrile technology, applied in the field of synthesis of high-yield salicylonitrile, can solve problems such as easy production of by-product benzoxazole, no phosgene treatment device, unfavorable industrial production, etc., and achieve production cost Low, stable product quality, and the effect of reducing the formation of by-products

Inactive Publication Date: 2016-11-09
ANHUI GUANGXIN AGROCHEM
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Problems solved by technology

However, this method is cumbersome to operate, the cost of raw materials is relatively expensive, the total yield of salicylonitrile is low, and a large amount of industrial wastes are generated, which is not conducive to industrial production
The second type of method is the ni

Method used

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Embodiment

[0020] The invention provides a kind of synthetic method of salicylonitrile with high yield. The synthetic method mainly comprises the following steps: (1) adding 1 mass part of salicylamide and 1.6 mass parts of solvent xylene into the reaction kettle, and opening the reaction kettle Stir fully; (2) After fully stirring, turn on the jacketed steam to slowly heat up the reactor, control the temperature of the reactor at 172°C, and feed phosgene at the same time to carry out the phosgenation reaction. The synthesis rate of cyanonitrile reduces the generation of by-products; (3) after the reaction is over, feed nitrogen into the reactor to get rid of the gas, and at the same time, an absorber can be set at the gas outlet of the reactor to absorb the mixed gas in the reactor in time , to avoid the leakage of toxic gas, the upper part of the absorber is equipped with an overflow pipe for distributing the absorption liquid, the absorption liquid in the overflow pipe is xylene, and t...

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Abstract

The invention provides a synthetic method for high-yield o-hydoxybenzonitrile. The synthetic method mainly comprises the following steps: 1) adding salicylamide and a solvent xylene in a reaction vessel, starting the reaction vessel for full stirring; 2) turning on a jacket for steam heating, simultaneously introducing phosgene for a reaction; 3) after the reaction is complete, introducing nitrogen for expelling gas, setting an absorber at a gas outlet of the reaction vessel; 4) transferring a mixture in the step 3) to a rectifying tower, respectively collecting the fraction with the temperature of 137-140 DEG C and 145-155 DEG C; 5) cooling the fraction with the temperature of 137-140 DEG C and distilling the fraction to obtain the solvent xylene; and 6) condensing the fraction with the temperature of 145-155 DEG C in the step 4) and slicing the fraction to obtain the product o-hydoxybenzonitrile. The method is mature and reliable, the product quality is high, the raw material consumption is low, the cost is low, compared with the same kind of the product, the content of the o-hydoxybenzonitrile is increased by 1.5%, and the impurity is decreased by 1.0%.

Description

technical field [0001] The invention relates to the synthesis of salicylonitrile, in particular to a high-yield synthesis method of salicylonitrile. Background technique [0002] Salicylonitrile, also known as o-hydroxybenzonitrile, is an off-white powdery solid with a very pungent odor. A small amount can affect people's breathing and has a bitter odor. Salicylonitrile is often used as an intermediate in the organic synthesis of Bunirolol and as an intermediate in the fungicide azoxystrobin. There are few reports about the synthesis of salicylonitrile, mainly following two types of reactions: [0003] The first type of reaction is that salicylaldehyde first generates salicylaldoxime with hydroxylamine hydrochloride, and then dehydrates with acetic anhydride or thionyl chloride to obtain salicylonitrile; [0004] The second type of reaction is the dehydration of salicylamide in the presence of phosgene or thionyl chloride or phosphorus oxychloride to obtain salicylonitrile...

Claims

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Application Information

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IPC IPC(8): C07C253/20C07C253/34C07C255/53
CPCC07C253/20C07C253/34C07C255/53
Inventor 黄金祥过学军吴建平胡明宏杨亚明程伟家李红卫徐小兵黄显超戴玉婷
Owner ANHUI GUANGXIN AGROCHEM
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