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Continuous preparation method of benzyl zinc halide and derivatives of benzyl zinc halide

A technology of benzyl zinc halide and derivatives, applied in the direction of zinc organic compounds, can solve the problems of inapplicability and scale-up production, and achieve the effect of avoiding the risk of spraying materials and improving contact efficiency

Active Publication Date: 2019-12-10
ASYMCHEM LAB TIANJIN
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The main purpose of the present invention is to provide a continuous preparation method of benzyl zinc halide and its derivatives, to solve the problem that the preparation method of benzyl zinc halide in the prior art is not suitable for scale-up production

Method used

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  • Continuous preparation method of benzyl zinc halide and derivatives of benzyl zinc halide
  • Continuous preparation method of benzyl zinc halide and derivatives of benzyl zinc halide
  • Continuous preparation method of benzyl zinc halide and derivatives of benzyl zinc halide

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preparation example Construction

[0023] As analyzed in the background technology of the present application, the technical scheme of direct insertion of zinc atoms into carbon-halogen bonds in the prior art is carried out by batch reaction, which is prone to material accumulation and causes the risk of material spraying, thus limiting its use in industrial scale-up production Applications. In order to solve the risk of spraying, metal magnesium / lithium chloride / zinc chloride was used to realize the insertion of zinc atoms in benzyl halohydrocarbons, but due to the solubility limitations of lithium chloride and zinc chloride in organic solvents , leading to the need for high-temperature processing, which also limits the application of this route in industrial scale-up production. In order to solve the problem that the preparation method of benzyl zinc halide in the prior art is not suitable for scale-up production, the application provides a continuous preparation method of benzyl zinc halide and derivatives t...

Embodiment 1

[0040] Under the protection of nitrogen, add 4.45Kg of tetrahydrofuran, 500g of 4-fluorochlorobenzyl, 18.8g of trimethylchlorosilane, and 32.5g of 1,2-dibromoethane into a 10L four-necked bottle, and stir for 10-20 minutes to form a liquid reaction materials.

[0041] use figure 1 The columnar reactor shown is for continuous reaction, wherein the temperature control range of the heating section 10 of the columnar reactor is 65-75°C, the temperature control range of the cooling section 20 is 15-25°C, and the product overflow port is set at the cooling The section 20 is close to one end of the heating section 10, the angle α between the drainage tube 21 and the outer wall is 25°, and the stirring speed is adjusted between 100-200r / min. Turn on the feed pump to provide the liquid reaction material to the heating section 10, and turn on the continuous solid feeder to provide the zinc powder to the heating section 10, wherein the flow rate of the liquid reaction material is contro...

Embodiment 2

[0043] Under the protection of nitrogen, add 4.45Kg of tetrahydrofuran, 500g of 4-fluorochlorobenzyl, 18.8g of trimethylchlorosilane, and 32.5g of 1,2-dibromoethane into a 10L four-necked bottle, and stir for 10-20 minutes to form a liquid reaction materials.

[0044] use figure 1 The columnar reactor shown is for continuous reaction, wherein the temperature control range of the heating section 10 of the columnar reactor is 65-75°C, the temperature control range of the cooling section 20 is 15-25°C, and the product overflow port is set at the cooling The section 20 is close to one end of the heating section 10, and the angle α between the drainage tube 21 and the outer wall is 40°. Turn on the feed pump to provide the liquid reaction material to the heating section 10, and turn on the continuous solid feeder to provide the zinc powder to the heating section 10, wherein the flow rate of the liquid reaction material is controlled to be 12g / min, and the zinc powder feeding rate ...

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Abstract

The invention provides a continuous preparation method of benzyl zinc halide and derivatives of the benzyl zinc halide. According to the continuous preparation method, a continuous reactor is adoptedfor the reaction that zinc atoms are directly insert into a carbon halogen bond, wherein, the continuous reactor includes a heating section and a cooling section which are arranged in a communicatingmode, the cooling section is located above the heating section, and the cooling section is provided with a product overflow port. The continuous preparation method comprises the steps that a liquid reaction material and zinc powder are continuously fed into the heating section, the zinc powder is continuously fed into the heating section from the upper part of the heating section, the liquid reaction material is continuously fed into the heating section from the lower part of the heating section, and the reaction that the zinc atoms are directly inserted into the carbon halogen bond is conducted in the heating section to obtain a product system, and the product system flows out of the continuous reactor from the product overflow port, wherein the liquid reaction material includes halide, and the halide has the structure formula I (please see the specifications for the formula I). According to the continuous preparation method, the zinc powder is not accumulated in the continuous reactor, thus the material spraying risk is avoided, and the continuous preparation method is applied to the enlarged production advantageously.

Description

technical field [0001] The invention relates to the actual preparation field of organic zinc, in particular to a continuous preparation method of benzyl zinc halide and derivatives thereof. Background technique [0002] Organozinc reagents are often used to construct organic molecules. Due to their unique chemical properties due to their good functional group compatibility and high reactivity, they are widely used in organic synthesis. Among the common organozinc reagents, benzylzinc reagent is an important benzyl functionalization reagent, which is often used to introduce benzyl groups into molecules. Functionalized benzylzinc halides occupy a unique position due to the high reactivity of benzyllithium and benzylmagnesium organometallic reagents, which make these organometallics easy to polymerize and unstable. [0003] Traditionally, the related benzylzinc halides are generated by batch reaction of active zinc and benzyl halides, and zinc atoms are directly inserted into ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F3/06
CPCC07F3/06
Inventor 洪浩卢江平丰惜春孙兴芳梁永
Owner ASYMCHEM LAB TIANJIN
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