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Continuous preparation method of o-chlorobenzyl chloride Grignard reagent

A technology of o-chlorobenzyl-Grignard and benzyl-chloro-Grigner, which is applied in the field of continuous preparation of o-chlorobenzyl-Grignard reagents, and can solve the problems of energy accumulation, large liquid holding capacity, and volume reduction, etc. , to achieve the effect of reducing side reactions, small liquid holding capacity of equipment, and reducing volume

Active Publication Date: 2020-05-12
HAILIR PESTICIDES & CHEM GRP
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to overcome the problem of triggering in the process of batch-type preparation of o-chlorobenzyl-clo-Grignard reagent in the prior art, the problems of poor heat transfer that easily lead to energy accumulation and potential safety hazards due to the large liquid holding capacity of the equipment Disadvantages, the technical solution of the present invention realizes the continuous preparation of o-chlorobenzyl chloride Grignard reagent by using a plurality of reactors connected in series, and the volume of a single reactor is reduced and the heat exchange area is increased by one initiation and continuous feeding, which improves the reaction rate. Excellent stability and safety, with the advantages of good heat transfer effect and small liquid holding capacity of equipment

Method used

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  • Continuous preparation method of o-chlorobenzyl chloride Grignard reagent
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  • Continuous preparation method of o-chlorobenzyl chloride Grignard reagent

Examples

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Effect test

Embodiment 1

[0030] A kind of continuous method for preparing the Grignard reagent of o-chlorobenzyl chloride, concrete steps are as follows: (3 reactors are connected in series)

[0031] Raw material preparation: add 700g of o-chlorobenzyl chloride and 2100g of ethylene glycol dimethyl ether into the raw material kettle, and mix well; add 100g and 25g of magnesium chips into the solid feeders of the two forward reaction kettles respectively for later use.

[0032]Carry out nitrogen flow purging to the whole reaction series system, and continue to pass nitrogen flow, add the ethylene glycol of ortho-chlorobenzyl chloride to the first reaction kettle (the reaction kettles are all 1000ml, and the effective volume to the overflow port is about 800ml). 100g of dimethyl ether solution (10g of o-chlorobenzyl chloride and 90g of ethylene glycol dimethyl ether), add 5g of magnesium chips, add 3 grains of iodine, and turn on the temperature control system so that the temperature of the first kettle ...

Embodiment 2

[0034] A kind of continuous method for preparing the Grignard reagent of o-chlorobenzyl chloride, concrete steps are as follows: (3 reactors are connected in series)

[0035] Raw material preparation: add 500g of o-chlorobenzyl chloride, 2000g of toluene, and 400g of tetrahydrofuran into the raw material kettle, and mix evenly; add 70g and 20g of magnesium chips into the solid feeders of the first two reaction kettles respectively for later use.

[0036] The whole reaction series system is purged with nitrogen flow, and the nitrogen flow is continued, and the toluene / tetrahydrofuran of o-chlorobenzyl chloride is added to the first reaction kettle (the reaction kettles are all 1000ml, and the effective volume to the overflow port is about 800ml). Solution 100g (wherein o-chlorobenzyl chloride is 10g, toluene is 75g, tetrahydrofuran 15g), adds 5g of magnesium chips, adds 3 grains of iodine, turns on the temperature control system, makes the temperature of the first still be 40 ℃,...

Embodiment 3

[0038] A kind of continuous method for preparing the Grignard reagent of o-chlorobenzyl chloride, concrete steps are as follows: (4 reaction kettles are connected in series)

[0039] Raw material preparation: add 1000g of o-chlorobenzyl chloride and 3000g of methyl tert-butyl ether into the raw material kettle, and mix well; add 125g, 45g and 15g of magnesium chips into the solid feeders of the three forward reaction kettles for later use.

[0040] The whole reaction series system is purged with nitrogen flow, and the nitrogen flow is continued, and in the first reaction kettle (the reaction kettles are all 1000ml, and the effective volume to the overflow port is about 800ml), the methyl tertiary methyl chloride of o-chlorobenzyl chloride is added. 100g of butyl ether solution (of which 10g of o-chlorobenzyl chloride and 90g of methyl tert-butyl ether), add 5g of magnesium chips, add 3 grains of iodine, and turn on the temperature control system so that the temperature of the f...

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Abstract

The invention relates to a continuous preparation method of an o-chlorobenzyl chloride Grignard reagent. The method specifically comprises the following steps: adding a mixed solution of o-chlorobenzyl chloride and a solvent into a reaction kettle, adding magnesium chips into reaction kettle, and carrying out a continuous reaction in a multi-kettle series connection mode, wherein the multi-kettleseries connection mode is specifically that n reaction kettles are connected in series, n is larger than or equal to 3, all the reaction kettles are provided with overflow ports, and the first reaction kettle to the (n-1) th reaction kettle are connected with the liquid inlet of the next stage of the reaction kettle through overflow pipelines. According to the technical scheme, a plurality of reaction kettles are connected in series to realize continuous preparation of an o-chlorobenzyl chloride Grignard reagent, the volume of a single reaction kettle is reduced and the heat exchange area is increased through one-time initiation and continuous feeding, the reaction stability and the safety are improved, and the method has the advantages of good heat transfer effect and small equipment liquid holdup.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a continuous preparation method of o-chlorobenzyl chloride Grignard reagent. Background technique [0002] O-chlorobenzyl Cloggard reagent is an important intermediate of fungicides prothioconazole and epoxiconazole, which is prepared by reacting o-chlorobenzyl chloride and magnesium. The molecular formula of o-chlorobenzyl chloride is C 7 h 6 Cl 2 Mg, its structural formula is: [0003] [0004] Prothioconazole is a new broad-spectrum triazolethione fungicide developed by Bayer. It has a unique triazolethione structure, not only has systemic activity, but also has excellent protection, treatment and eradication activities. It is mainly used to prevent and control many diseases of crops such as cereals, wheat and beans; prothioconazole not only has good safety for crops, but also has the advantages of good control effect, long-lasting effect and obvio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F3/02
CPCC07F3/02
Inventor 王旭李建国毕旌富王凯矫立鹏周先峰栾明奎
Owner HAILIR PESTICIDES & CHEM GRP
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