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A kind of method of synthesizing phthalic dimethanol derivative

A technology for ortho-phthalic alcohol and derivatives, applied in the field of synthesizing ortho-phthalic alcohol derivatives, can solve the problems of high requirements for reaction equipment, difficult sources of reaction raw materials, expensive hydrogenation catalysts, etc. Easy storage, preparation process and product separation and purification

Active Publication Date: 2021-07-23
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The problem in the technique of the method for synthesizing phthalic dimethanol derivatives in the above-mentioned method is that the source of reaction raw materials using ortho-dichloromethylbenzene is difficult to synthesize and is irritating. Environmental protection; the hydrogenation reduction method requires the use of expensive hydrogenation catalysts and high reaction pressure, which requires high reaction equipment; the method using phthalic acid (ester) or phthalide as raw material needs to use water-sensitive Strong reducing agent BH 3 -Me 2 S, LiBH 4 or LiAlH 4 , the process conditions are harsh, and the cost is high

Method used

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  • A kind of method of synthesizing phthalic dimethanol derivative
  • A kind of method of synthesizing phthalic dimethanol derivative
  • A kind of method of synthesizing phthalic dimethanol derivative

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Synthesis of o-phthalmethanol:

[0024]

[0025] Put phthalide (0.4 mmol), potassium hydroxide (0.4 mmol), phenylsilane (1.2 mmol) and tetrahydrofuran (4 mL) into the reaction flask, react at 66°C for 4 h, stop the reaction, add a small amount of alcohol dropwise to quench the reaction, After separation, 54 mg of o-phthalamide was obtained, with a yield of 98%.

Embodiment 2

[0026] Example 2 Put phthalide (0.4 mmol), sodium hydroxide (0.4 mmol), diphenylsilane (1.6 mmol) and tetrahydrofuran (4 mL) into the reaction flask, react at 66°C for 4 h, stop the reaction, add a small amount of The reaction was quenched with alcohol, and 44 mg of o-phthalyl dimethanol was obtained after separation, with a yield of 80%.

Embodiment 3

[0027] Example 3 Put phthalide (0.4 mmol), potassium hydroxide (0.4 mmol), triphenylsilane (1.6 mmol) and tetrahydrofuran (4 mL) into the reaction flask, react at 66°C for 6 h, stop the reaction, add a small amount of The reaction was quenched with alcohol, and 43 mg of o-phthalyl dimethanol was obtained after separation, with a yield of 78%.

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Abstract

The invention belongs to the technical field of chemical industry, and specifically relates to a method for synthesizing o-phthalamide derivatives. The invention uses phthalide as a raw material, and under the action of an alkali and a silane compound, undergoes a reductive ring-opening reaction to prepare o-phthalamide. The method of the invention has easy-to-obtain raw materials, simple and convenient operation, strong reaction selectivity, high product yield and mild reaction conditions; the synthesized mono- or multi-substituted phthalic dimethanol derivatives have high quality and good functional group compatibility.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a method for synthesizing o-phthalamide derivatives. Background technique [0002] O-phthalmethanol is an important class of organic synthesis intermediates, which can be used to prepare fine chemicals and pharmaceutical intermediates, etc., and it can also be used as resin additives, and has a wide range of applications. [0003] In the existing preparation technology, there are many reports on the synthesis of o-phthalamide derivatives, mainly including the preparation method reported in the literature (CN201010568813.2) that uses o-dichloromethylbenzene as a raw material and undergoes a hydrolysis reaction in an alkaline environment ; The document (CN 201410724375.2) reported that phthalic anhydride containing halogenated alkanes was used as a raw material, and hydrogenation reaction occurred in the presence of a hydrogenation catalyst under the condition...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/147C07C33/26C07C201/12C07C205/19C07C253/30C07C255/53
CPCC07C29/147C07C201/12C07C253/30C07C33/26C07C205/19C07C255/53
Inventor 周锡庚刘斌张德兴王圣克
Owner FUDAN UNIV