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Preparation method of borphenyl pyridine

A technology of triphenylboron pyridine and tetraphenylboron chloride, which is applied in the field of simple synthesis of a new type of organoboron fungicide - triphenylboron pyridine, can solve the problems of limited use of solvents, difficult control of product purity, uneven heating, etc. , to achieve the effect of low cost, high product purity and simple process

Inactive Publication Date: 2013-07-10
SHIJIAZHUANG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The solvents used in the synthesis process are complex solvents, which limits the use of recovered solvents
Tetraphenylboron pyridine is heated and debenzene is carried out under a single solid, and the purity of the product is difficult to control due to inhomogeneous heating

Method used

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  • Preparation method of borphenyl pyridine
  • Preparation method of borphenyl pyridine
  • Preparation method of borphenyl pyridine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Embodiment 1: a kind of preparation method of triphenylboron pyridine is realized by the following steps:

[0036] The input amount of each substance used in the preparation is based on trimethyl borate / mL=(15.8-19.3) as the standard, the solid is measured by mass, and the liquid is measured by volume.

[0037] (1) Preparation of Phenylmagnesium Chloride (Grignard Reagent) Add 16.0g of magnesium powder and 0.1g of iodine to a 500mL three-necked flask equipped with a reflux condenser (top-mounted tee), dropping funnel and magnetic stirring, and use For argon replacement, first add 2.5mL bromobenzene and 40mL tetrahydrofuran (THF) into the reaction flask, and stir until the reaction is initiated (the color of iodine disappears and a large amount of heat is released). Add 66.0 mL of chlorobenzene and 160.0 mL of tetrahydrofuran into the dropping funnel. After the oil bath was heated to 70°C, the mixed solution of chlorobenzene and tetrahydrofuran was slowly added dropwise...

Embodiment 2

[0051] Embodiment 2: a kind of preparation method of triphenylboron pyridine is realized by following steps:

[0052] The input amount of each substance used in the preparation is based on trimethyl borate / mL=(15.8-19.3) as the standard, the solid is measured by mass, and the liquid is measured by volume.

[0053] (1) Preparation of Phenylmagnesium Chloride (Grignard Reagent) Add 16.0g of magnesium powder and 0.1g of iodine to a 500mL three-necked flask equipped with a reflux condenser (top-mounted tee), dropping funnel and magnetic stirring, and use For argon replacement, first add 2.5mL bromobenzene and 40mL tetrahydrofuran (THF) into the reaction flask, and stir until the reaction is initiated (the color of iodine disappears and a large amount of heat is released). Add 66.0 mL of chlorobenzene and 160.0 mL of tetrahydrofuran into the dropping funnel. After the oil bath was heated to 60°C, the mixed solution of chlorobenzene and tetrahydrofuran was slowly added dropwise for...

Embodiment 3

[0067] Embodiment 3: a kind of preparation method of triphenylboron pyridine is realized by following steps:

[0068] The input amount of each substance used in the preparation is based on trimethyl borate / mL=(15.8-19.3) as the standard, the solid is measured by mass, and the liquid is measured by volume.

[0069] (1) Preparation of Phenylmagnesium Chloride (Grignard Reagent) Add 16.0g of magnesium powder and 0.1g of iodine to a 500mL three-necked flask equipped with a reflux condenser (top-mounted tee), dropping funnel and magnetic stirring, and use For argon replacement, first add 2.5mL bromobenzene and 40mL tetrahydrofuran (THF) into the reaction flask, and stir until the reaction is initiated (the color of iodine disappears and a large amount of heat is released). Add 66.0 mL of chlorobenzene and 160.0 mL of tetrahydrofuran into the dropping funnel. After the oil bath was heated to 40°C, a mixed solution of chlorobenzene and tetrahydrofuran was slowly added dropwise for 3...

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Abstract

The invention discloses a preparation method of borphenyl pyridine. The method comprises the following steps: A, preparing phenylmagnesium chloride; B, synthesizing tetraphenyl boric magnesium chloride; C, synthesizing sodium tetraphenylborate; D, synthesizing pyridine hydrochloride; E, synthesizing tetrapheny boron pyridine; and F, synthesizing the borphenyl pyridine. The synthesizing diagram is shown in the specification. The method can be used for easily preparing a final product with high purity and good yield. The method has the characteristics of being simple in process, low in cost and high in product purity.

Description

technical field [0001] The invention relates to a convenient synthesis method of a novel organoboron fungicide-triphenylboron pyridine, belonging to the technical field of chemical synthesis. Background technique [0002] Although there are other methods of dock preservation, the traditional application of biocides still dominates. The fungicides used in marine coatings in the past were organotin compounds (tributyltin, TBT), which pollute the sea. In 2004, the researchers of Invasta Corporation (Invasta) launched the commercialized product Borocide brand, which is a boron-containing biocide based on triphenylboron pyridine. It can be decomposed into non-toxic substances and can be used in marine coatings. In the prior art, the new method (JP 2003238572, 2003) adopted by Hokko Chemical Industry Co., Ltd. is a practical industrial method. The synthesis of their triphenylboron pyridine needs to use pure sodium tetraphenylborate, which increases the synthesis cost. The solv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/02
Inventor 刘树彬李志安张雪红郧海丽
Owner SHIJIAZHUANG UNIVERSITY
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