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Preparation method for ditertbutyl dicarbonate

A technology of di-tert-butyl ester and dicarbonic acid, which is applied in the field of preparation of di-tert-butyl dicarbonate, can solve the problems of insufficient reactivity, large pollution, low purity, etc., and achieves improved reaction temperature, high safety and simple process. Effect

Active Publication Date: 2012-02-15
THE IT ELECTRONICS ELEVENTH DESIGN & RES INST SCI & TECHNOLOGICAL ENG
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Problems solved by technology

The synthetic method of di-tert-butyl dicarbonate mainly contains at present: (1) metal potassium phosgene method, and this method cost is high
(2) Sodium metal plus benzoyl chloride method, this method has large pollution, low purity and insufficient reactivity
(3) The patent number is "ZL200610086299.2, and the patent name is: the preparation method of di-tert-butyl dicarbonate". This method directly uses sodium tert-butoxide mixed with n-hexane for reaction, and its dispersibility and activity are not enough. The yield very low

Method used

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Embodiment Construction

[0012] Below we will further illustrate the present invention in conjunction with embodiment.

[0013] (1) Catalyst preparation: Dissolve 238g of nickel chloride, 133g of aluminum trichloride, 270g of ferric chloride and 170g of copper chloride in 4055g of hot absolute alcohol, the temperature of the absolute alcohol is 70°C; after the dissolution is complete, add 811g of activated carbon for coconut shell injection was evenly stirred and poured into an evaporating dish and placed in a vacuum oven, baked at a constant temperature for 5 hours at a temperature of 120° C., cooled and crushed to obtain a catalyst.

[0014] (2) Synthesis of sodium tert-butoxide: Add 1500g of organic solvent toluene to 500g of anhydrous tert-butanol, add 10g of the catalyst prepared in step (1) and 260g of sodium amide at the same time and react at 90°C for 8 hours to obtain tert-butyl Sodium alkoxide solution.

[0015] (3) Carbonylation reaction: Lower the temperature of the sodium tert-butoxide s...

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Abstract

The invention discloses a preparation method for ditertbutyl dicarbonate. In the method, the ditertbutyl dicarbonate is prepared from self-made sodium tert-butoxide solution, diphosgene and a catalyst under a certain condition. The preparation method has the advantages of simple process, high yield, high purity, capability of raising reaction temperature by substituting normal hexane with toluene(normal hexane is used in the conventional method) and higher safety.

Description

technical field [0001] The invention relates to the field of fine chemical synthesis, in particular to a preparation method of di-tert-butyl dicarbonate. Background technique [0002] Di-tert-butyl dicarbonate, also known as BOC anhydride, is used to introduce tert-butoxycarbonyl protection genes in organic synthesis, especially for the amino protection of amino acids. It is widely used in the synthesis of various products such as medicine, protein and peptide synthesis, biochemical food, cosmetics, etc. Di-tert-butyl dicarbonate is a new type of amino acid protective agent, which is safer, more economical, more efficient and easier than traditional protective agents (such as benzyl chloroformate, chloroformic acid-P-fluorenic acid, etc.) control. The synthetic method of di-tert-butyl dicarbonate mainly contains at present: (1) metal potassium phosgene method, and this method cost is high. (2) Sodium metal plus benzoyl chloride method, this method is polluting, the purity...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/96C07C68/04
Inventor 赵振元罗明树
Owner THE IT ELECTRONICS ELEVENTH DESIGN & RES INST SCI & TECHNOLOGICAL ENG
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