Synthetic method of di-tert-butyl dicarbonate

A technique for the synthesis of di-tert-butyl ester, which is applied in the preparation of carbon dioxide or inorganic carbonate, organic chemistry, reagents, etc., can solve the problems of cumbersome production steps, high risk factor, difficult product purification, etc., and achieve convenient solvent recovery and treatment , Simplify the experimental steps, and reduce the production cost

Inactive Publication Date: 2017-05-31
SHANDONG JINCHENG KERUI CHEMICAL CO LTD
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Problems solved by technology

[0006] The purpose of the present invention is to provide a synthesis method of di-tert-butyl dicarbonate, which solves the problems of cumbersome production steps, high risk factor and difficult ...

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  • Synthetic method of di-tert-butyl dicarbonate

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Embodiment 1

[0020] The synthetic method of di-tert-butyl dicarbonate is as follows:

[0021] (1) use N 2 Empty the autoclave with a capacity of 2L, add 85g of tert-butanol, 650g of n-hexane, and 25g of sodium metal successively, heat to 110°C, and stir rapidly. At this time, the pressure in the autoclave is about 0.2MPa. React for 5-6 hours, and when there is no change in the pressure in the kettle for 15 minutes, the preparation of sodium tert-butoxide is completed;

[0022] (2) Cool down to -5 ~ 5 ℃, open the vent valve, and introduce CO 2 , until CO 2 No more absorption, continue to stir for 20 minutes after ventilation, keep the temperature constant, add 1g of pyridine, dissolve triphosgene with 65g of n-hexane, and then add it dropwise into the reaction kettle for about 3 to 4 hours, keep the temperature constant, - Insulate at 5-5°C for 1 hour, raise the temperature to 25-30°C and hold for 2 hours, remove the solvent at 80-90°C under normal pressure (whether it refers to distilla...

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Abstract

The invention relates to a synthetic method of di-tert-butyl dicarbonate, and belongs to the technical field of synthesis and purification of chemical engineering products. The synthetic method comprises the following steps: adding tert-butanol, n-hexane and metal sodium to an autoclave under the protection of nitrogen to obtain sodium tert-butoxide, introducing CO2, stirring the sodium tert-butoxide, adding a catalyst, dropwise adding triphosgene dissolved in n-hexane to the autoclave, carrying out a heat insulation reaction, carrying out reduced pressure distillation to remove the n-hexane, adding water, washing the obtained reaction product, layering the washed reaction product, taking the above obtained organic phase, and carrying out cooling, freeze crystallization, centrifuge and drying to obtain the di-tert-butyl dicarbonate. The di-tert-butyl dicarbonate is prepared from the sodium tert-butoxide, a single solvent is used, experiment steps are simplified, normal pressure solvent removal is carried out after the reaction, and water washing is carried out, so the use amount of a dehydrating agent is reduced, water in the solvent is controlled, and the solvent recovery treatment is convenient; and triphosgene is highly-efficiently and easily degraded, and the catalyst is cheap and is easy to obtain, so the production cost is reduced, and the reaction efficiency is improved.

Description

technical field [0001] The invention relates to a method for synthesizing di-tert-butyl dicarbonate, belonging to the technical field of synthesis and purification of chemical products. Background technique [0002] Di-tert-butyl dicarbonate, referred to as Diboc, the molecular formula is C 10 h 18 o 5 , the structural formula is as follows: [0003] [0004] Diboc is a white crystalline solid or colorless transparent liquid, easily soluble in organic solvents such as benzene, xylene, n-hexane, and insoluble in water. It is an important amino acid protective agent with the advantages of high activity and low price. The product is isobutene and CO 2 , will not cause new pollution. [0005] At present, the preparation process of Diboc is mainly to prepare sodium tert-butoxide or potassium tert-butoxide by reacting metal sodium or potassium with tert-butanol in a high boiling point solvent, and react with diphosgene or phosgene to form Diboc after removing the solvent. ...

Claims

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Application Information

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IPC IPC(8): C07C69/96C07C68/04
CPCC07C68/04C07C69/96Y02P20/141
Inventor 郑庚修孙智源张林
Owner SHANDONG JINCHENG KERUI CHEMICAL CO LTD
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