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Preparation method of high-purity chloro-2-carboxyl-benzophenone

A technology of methyl benzophenone and benzophenone is applied in the preparation of carboxylate, the preparation of carbon-based compounds, the preparation of organic compounds, etc., to achieve the effects of environmental protection, high purity and simple synthesis steps

Active Publication Date: 2018-09-14
王华平
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

2-Carboxyl benzophenone has some synthetic methods reported (Journal of the American Chemical Society, 36,732-7; 1914), this type of method is mainly obtained by the Friedel-Crafts reaction of benzene and phthalic anhydride, but for aromatic rings with substituents Synthesis of benzophenone compounds such as chlorinated 2-carboxybenzophenone is not covered

Method used

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  • Preparation method of high-purity chloro-2-carboxyl-benzophenone
  • Preparation method of high-purity chloro-2-carboxyl-benzophenone
  • Preparation method of high-purity chloro-2-carboxyl-benzophenone

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preparation example Construction

[0028] The preparation method reaction scheme of the present invention is as follows:

[0029]

[0030] Take 2-chloro-6-(2-chlorobenzoyl)benzoic acid (compound A) and 6-(2-chlorobenzoyl)benzoic acid (compound B) as an example to illustrate the technical scheme of the present invention,

[0031]

Embodiment 1

[0032] The preparation of embodiment 1 compound A (2-chloro-6-(2-chlorobenzoyl) benzoic acid)

[0033] (1) Preparation of Grignard Reagents

[0034]

[0035] Get 24 grams (1.0M) of magnesium powder, put into four-neck round bottom flask, pass into dry hot nitrogen, cool after 30 minutes. Add 2-methyl m-dichlorobenzene, a small amount of tetrahydrofuran and iodine, and heat to initiate the reaction. Add tetrahydrofuran agent dropwise to the reaction bottle to make the total solvent volume 1000 ml, control the reaction temperature, react for 4 hours, cool, and the obtained Grignard reagent is ready for use.

[0036] (2) Preparation of intermediate 2-chloro-6-(2-chlorobenzoyl)toluene

[0037]

[0038] 1000 ml of tetrahydrofuran solution (concentration 1.0 M) of Grignard reagent was slowly dropped into toluene solution containing 350.0 g (2.0 M) o-chlorobenzoyl chloride under ice-bath conditions, and the reflux reaction was continued for 24 hours. After the reaction was co...

Embodiment 2

[0041] The preparation of embodiment 2 compound B (6-(2-chlorobenzoyl) benzoic acid)

[0042] (1) Preparation of Grignard Reagents

[0043]

[0044] Get 48 grams (2.0M) of magnesium powder, put into four-neck round bottom flask, pass into dry hot nitrogen, cool after 30 minutes. Add o-methyl chlorobenzene, a small amount of ether and iodine, and heat to initiate the reaction. Diethyl ether was added dropwise to the reaction bottle to make the total solvent volume 1000 ml, the reaction temperature was controlled, the reaction was carried out for 4 hours, cooled, and the obtained Grignard reagent was used for future use.

[0045] (2) Preparation of intermediate 6-(2-chlorobenzoyl) toluene

[0046]

[0047] Add 1000 ml of ether solution (concentration 2.0M) of Grignard reagent into the xylene solution containing 420.0 g (2.4M) o-chlorobenzoyl chloride slowly under ice-bath conditions, and continue the reflux reaction for 36 hours. After the reaction is completed, depressu...

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Abstract

The invention discloses a preparation method of high-purity chloro-2-carboxybenzophenone. The preparation method comprises the following steps: preparing chlorine-substituted or non-substituted o-chlorotoluene into a Grignard reagent, and then, enabling the Grignard reagent to react with o-chlorobenzoyl chloride to obtain chloro-2-methylbenzophenone; and enabling chloro-2-methylbenzophenone to besubjected to oxidation reaction in the presence of a catalyst and an oxidizing agent to obtain the chloro-2-carboxybenzophenone. The preparation method disclosed by the invention has the advantages that the synthetic steps are simple, the cost is low, the process is environmentally friendly, and the obtained product has high purity and can be directly applied to the fields of micro-electronics andthe like.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a new synthesis process of a class of high-purity chlorinated benzophenones. Background technique [0002] Benzophenones belong to a large family in the world of chemical substances, and are widely used in medicine, pesticides, dyes, plastics, coatings, daily chemicals, electronic chemicals and other fields. For example, benzophenone derivatives, as the pharmacophore of non-steroidal anti-inflammatory drugs, have become a class of widely used drug intermediates. Benzophenone-based photoinitiators are currently the most productive photoinitiators due to their high quantum efficiency. In the electronics industry, aminobenzophenones have good semiconductor frequency doubling functions. In all fields, the most widely used category is ultraviolet absorbers, which can be used in the preparation of sunscreen oil or sunscreen cream in the cosmetics industry. Carboxylic ben...

Claims

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Application Information

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IPC IPC(8): C07C65/105C07C51/265C07C51/43C07C45/45C07C49/813C07F3/02
CPCC07C45/455C07C51/265C07C51/43C07F3/02C07C49/813C07C65/105
Inventor 王华平
Owner 王华平
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