阅读说明：本技术 一种对氰基氯苄的合成方法 (A kind of synthetic method of pair of cyano benzyl chloride ) 是由 吴水保 于 2018-05-25 设计创作，主要内容包括：本发明公开了一种对氰基氯苄的合成方法,包括以下步骤：(1)取20mL对二甲基苯置于反应釜中,将反应釜加热至130-135℃,依次加入溶剂DMF、催化剂及助催化剂,控制氧气通入量为900mL/min,氢气通入量为100mL/min,反应4-5h；(2)将上述反应液降温至室温,得到的透明无色晶体即为对甲基苯甲腈,使用DMF将得到的晶体洗涤2-3次后,抽滤除去DMF溶剂即可得到纯度高于90%的对甲基苯甲腈；(3)向对甲基苯甲腈中通入氯气,往反应器中通入光源,得到的白色针状结晶即为对氰基氯苄；本发明收率高,产品的纯度高,对设备的要求低,为对氰基氯苄的工业化生产提供了一条更为经济和环保的新途径。(The invention discloses the synthetic methods of a kind of pair of cyano benzyl chloride, the following steps are included: (1) takes 20mL to be placed in reaction kettle dimethyl benzene, reaction kettle is heated to 130-135 DEG C, sequentially add solvent DMF, catalyst and co-catalyst, control oxygen intake is 900mL/min, hydrogen intake is 100mL/min, reacts 4-5h；(2) above-mentioned reaction solution is cooled to room temperature, obtained clear colorless crystals be to methyl benzonitrile, after obtained crystal is washed 2-3 time using DMF, filter remove DMF solvent can be obtained purity be higher than 90% to methyl benzonitrile；(3) it is passed through chlorine in methyl benzonitrile, light source is passed through into reactor, obtained white, needle-shaped crystals are to cyano benzyl chloride；High income of the present invention, the purity is high of product, the requirement to equipment is low, provides a new way more economical and environmentally friendly for the industrialized production to cyano benzyl chloride.)

1. the synthetic method of a kind of pair of cyano benzyl chloride, it is characterised in that the following steps are included:

(1) it takes 20mL to be placed in reaction kettle dimethyl benzene, reaction kettle is heated to 130-135 DEG C, sequentially add solvent N, N- The additional amount of dimethylformamide DMF, catalyst and co-catalyst, the n,N-Dimethylformamide DMF is 20-25mL, is urged Agent and the additional amount of co-catalyst are respectively 2.0-3.0g and 10-15g, and control oxygen intake is 900mL/min, and hydrogen is logical Entering amount is 100mL/min, reacts 4-5h；

(2) above-mentioned reaction solution is cooled to room temperature, obtained clear colorless crystals are to be incited somebody to action using DMF methyl benzonitrile After the crystal that arrives washs 2-3 time, filter remove DMF solvent can be obtained purity be higher than 90% to methyl benzonitrile；

(3) to above-mentioned to chlorine is passed through in methyl benzonitrile, light source is passed through into reactor, outlet density is controlled in 0.97- 0.98, after reacting 4-5h, obtained white, needle-shaped crystals are to cyano benzyl chloride.

2. the synthetic method of a kind of pair of cyano benzyl chloride according to claim 1, it is characterised in that: urged in the step (1) Agent and the molar ratio of co-catalyst are 1:10.

Technical field

The present invention relates to technical field of organic synthesis, the synthetic method of specifically a kind of pair of cyano benzyl chloride.

Background technique

To cyano benzyl chloride also known as 4- (chloromethyl) benzonitrile, English entitled 4- (Chloromethyl) benzonitrile, Molecular formula is C₈H₆ClN, molecular weight 151.5929, CAS registration number is 874-86-2, for synthesizing talan fluorescent brightening Agent, while can be also widely applied to dyestuff, pesticide, synthetic perfume, detergent, dyeing auxiliaries, plasticizer, synthetic resin etc..

Due to benzyl chloride can derive it is a series of have in higher economic value to body or fine chemicals, while chlorine The chlorine of alkali factory can be balanced by changing benzyl production, thus benzyl chloride production is paid attention in the whole nation by chlor-alkali enterprises.Currently, benzyl chloride produces There are many method, mainly there is benzyl alcohol chloro method, chloromethylation process, toluene catalytically chloridising etc..But above-mentioned reaction method is due to anti- Answer process complicated, the waste liquid of generation is difficult to handle, it is at high cost the disadvantages of, cause the above method to be difficult to be promoted.

Therefore, for problems existing for above-mentioned synthetic method, the synthetic method for researching and developing a kind of pair of cyano benzyl chloride is this The very urgent requirement of industry.

Summary of the invention

The purpose of the present invention is to many deficiencies existing for the above-mentioned synthetic method to cyano benzyl chloride, provide a kind of comprehensive Conjunction cost of material is low, safety coefficient is high, the three wastes are easily processed, step is few, the synthetic method to cyano benzyl chloride of high income.

The present invention provides the synthetic methods of a kind of pair of cyano benzyl chloride, comprising the following steps:

(1) it takes 20mL to be placed in reaction kettle dimethyl benzene, reaction kettle is heated to 130-135 DEG C, sequentially add solvent N, N- The additional amount of dimethylformamide DMF, catalyst and co-catalyst, the n,N-Dimethylformamide DMF is 20-25mL, is urged Agent and the additional amount of co-catalyst are respectively 2.0-3.0g and 10-15g, and control oxygen intake is 900mL/min, and hydrogen is logical Entering amount is 100mL/min, reacts 4-5h；

(2) above-mentioned reaction solution is cooled to room temperature, obtained clear colorless crystals are to be incited somebody to action using DMF methyl benzonitrile After the crystal that arrives washs 2-3 time, filter remove DMF solvent can be obtained purity be higher than 90% to methyl benzonitrile；

(3) to above-mentioned to chlorine is passed through in methyl benzonitrile, light source is passed through into reactor, outlet density is controlled in 0.97- 0.98, after reacting 4-5h, obtained white, needle-shaped crystals are to cyano benzyl chloride.

Preferably, the molar ratio of catalyst and co-catalyst is 1:10 in heretofore described step (1).

The present invention passes through liquid-phase ammoxidation one-step synthesis method under paraxylene normal pressure and recycles methyl benzonitrile to methyl Benzonitrile and chlorine reaction are generated to cyano benzyl chloride, and high income, the purity is high of product, the requirement to equipment is low, are paraxylene Selective oxidation synthesis provides a new way more economical and environmentally friendly to the industrialized production of cyano benzyl chloride.

Specific embodiment