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Method for synthesizing o-benzenedicarbinol derivative

A technology for ortho-phthalic alcohol and derivatives, which is applied in the field of synthesizing ortho-phthalic alcohol derivatives, can solve the problems of difficult source of reaction raw materials, high requirements for reaction equipment, expensive hydrogenation catalysts, etc., and meets the requirements of easy transportation, storage, and equipment. The effect of low, simple preparation process and product separation and purification

Active Publication Date: 2018-10-02
FUDAN UNIV
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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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  • Method for synthesizing o-benzenedicarbinol derivative
  • Method for synthesizing o-benzenedicarbinol derivative
  • Method for synthesizing o-benzenedicarbinol derivative

Examples

Experimental program
Comparison scheme
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 engineering and particularly relates to a method for synthesizing an o-benzenedicarbinol derivative. Phthalide as a raw material is subjected to a reduction ring-opening reaction under the action of alkali and silane compounds, and o-benzenedicarbinol is prepared. According to the method, raw materials are easy to obtain, the method is simple and convenient to operate, the reaction selectivity is high, the product yield is high, and the reaction condition is mild; the synthesized monosubstituted or polysubstituted o-benzenedicarbinol derivative has 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 Applications(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
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