Preparation method of di-tert-butyl dicarbonate

A technology of di-tert-butyl ester and dicarbonic acid, applied in the field of preparation of di-tert-butyl dicarbonate, can solve the problems of unenvironmental protection, difficult purification, and high production cost, and achieve the effects of reducing waste water volume, simple process and reducing production cost.

Inactive Publication Date: 2017-06-13
SHANDONG JINCHENG KERUI CHEMICAL CO LTD
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a preparation method of di-tert-butyl dicarbonate, which solves the problems of high production cost, difficult purification, non-environmental protection and potential safety hazards in the current technology, and has the advantages of simple process route, low production cost, Features of safety and environmental protection

Method used

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Examples

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Embodiment 1

[0022] The preparation method of di-tert-butyl dicarbonate comprises the following steps:

[0023] (1) Synthesis of sodium tert-butoxide: add 20g sodium metal to 400g xylene, heat to 130-140°C to obtain sodium sand, slowly add 95-96g tert-butanol dropwise at this temperature to obtain sodium tert-butoxide The solution was cooled to below 5°C and suction filtered to obtain sodium tert-butoxide, and the mother liquor was applied mechanically;

[0024] (2) Dissolve the prepared sodium tert-butoxide in petroleum ether, and pass through carbon dioxide at -5 to 10°C for 3 hours to react. After the reaction is completed, a monoester sodium salt solution is obtained;

[0025] (3) Add 2g of N,N-dimethylformamide, 1g of pyridine, and 1g of triethylamine to the monoester sodium salt solution, cool down to -5~0°C, slowly add 60g of diphosgene dropwise, drop in 1.5h After the addition was completed, the temperature was raised to room temperature (25°C), and the reaction was kept for 2 hou...

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Abstract

The invention relates to a preparation method of di-tert-butyl dicarbonate and belongs to the technical field of synthesis of pharmaceutical intermediates. The preparation method comprises the following steps: adding metal sodium into xylol; heating to obtain sodium sand; then dropwise adding tert-butyl alcohol and carrying out pumping filtration to obtain sodium tert-butoxide; dissolving the sodium tert-butoxide into petroleum ether; introducing carbon dioxide and reacting to obtain a monoester sodium salt solution; adding a catalyst and slowly dropwise adding diphosgene to react; after reacting, standing and carrying out the pumping filtration; and washing with water, drying, distilling, cooling and crystallizing to obtain the di-tert-butyl dicarbonate. According to the preparation method, the sodium tert-butoxide is prepared from the metal sodium and the di-tert-butyl dicarbonate is prepared from the sodium tert-butoxide; a pumping filtration method is used for replacing a previous distillation method, so that the process is simpler and more energy is saved; the petroleum ether is used for replacing n-hexane and toluene, so that the production cost is reduced and a product is easier to purify; and finally, after the reaction, the pumping filtration is carried out and then water washing is carried out, so that the amount of wastewater is reduced and the environment-friendly treatment cost is reduced.

Description

technical field [0001] The invention relates to a preparation method of di-tert-butyl dicarbonate, belonging to the technical field of pharmaceutical intermediate synthesis. Background technique [0002] Di-tert-butyl dicarbonate, also known as BOC anhydride, is a new type of amino protecting agent, which is used to introduce tert-butoxycarbonyl protecting agent in organic synthesis, especially for the amino protection of amino acids, and is widely used in medicine, protein And in the synthesis of various products such as peptides, biochemistry, food, cosmetics, etc. At present, the synthesis of di-tert-butyl dicarbonate mainly contains the following methods: [0003] (1) metal sodium adds triphosgene method, the production cost of this method is low, but triphosgene is solid, is difficult for feeding intake, has increased the risk of suitability for industrialized production; [0004] (2) sodium tert-butoxide is mixed with n-hexane for reaction. After the reaction is comp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C68/04C07C69/96
CPCC07C29/70C07C68/04C07C69/96C07C31/30Y02P20/141
Inventor 郑庚修孙智源赵建国
Owner SHANDONG JINCHENG KERUI CHEMICAL CO LTD
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