Method for preparing di-tert-butyl dicarbonate

A technology of di-tert-butyl and dicarbonic acid, which is applied in the field of preparation of di-tert-butyl dicarbonate, can solve the problems of difficult product purification, low reaction yield, large dosage, etc., and achieve good product purity, convenient process operation, The effect of less waste

Active Publication Date: 2007-02-21
宁夏金象医药化工有限公司
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Problems solved by technology

The modified method to produce di-tert-butyl dicarbonate requires a large amount of aromatic or alipha

Method used

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  • Method for preparing di-tert-butyl dicarbonate

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specific example 1

[0025] Add 40g of sodium tert-butoxide into a 500ml four-neck flask, then add 320ml of n-hexane and stir. When the temperature drops to 12°C, start to introduce carbon dioxide, and keep warm for 1 hour after aeration. Add the catalyst, add 21g of Shuangguang in batches at 15°C, keep warm for 2 hours after the addition, and then take samples for analysis. After the reaction was completed, 100ml of water was added, stirred for 30 minutes, the lower water phase was separated, the oil phase was filtered, and the filtrate was concentrated, crystallized, and suction filtered to obtain a white crystalline solid. Dry under reduced pressure to obtain 25 g of the product di-tert-butyl dicarbonate.

specific example 2

[0027] Add 40g of sodium tert-butoxide into a 500ml four-necked bottle, then add 320ml of n-hexane and stir. When the temperature drops to 12°C, start to feed carbon dioxide, and keep warm for 1 hour after ventilation. Add the catalyst, add 20.5g Sanko in batches at 15°C, keep the temperature for 2 hours after the addition, and then take samples for analysis. After the reaction was completed, 100ml of water was added, stirred for 30 minutes, the lower water phase was separated, the oil phase was filtered, and the filtrate was concentrated, crystallized, and suction filtered to obtain a white crystalline solid. Dry under reduced pressure to obtain 26 g of di-tert-butyl dicarbonate.

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Abstract

This invention discloses a method for preparing di-tert-butyl dicarbonate. The method comprises: (1) stirring sodium tert-butoxide and hexane for cooling; (2) introducing CO2, and keeping the temperature at 5-15 deg.C; (3) adding bis(trichloromethyl) carbonate or trichloro methyl chloroformate; (4) keeping the temperature, and adjusting the pH to 5-6; (5) adding water, keeping the temperature at 0-5 deg.C, stirring and wshing with water to neutrality; (6) removing the solvent under normal pressure to 80-90 deg.C, and cooling to room temperature; (7) freezing and crystallizing; (8) separating and drying by centrifuging; (9) placing the dried material in a kettle, keeping the temperature at 25-30 deg.C, stirring, evacuating to -0.095 MPa, discharging and storing at -5-10 deg.C. The method uses chloroformate as a substitute for sulfuryl chloride, thus has such advantages as easy operation, little waste, high yield and high product purity, and is suitable for mass production.

Description

technical field [0001] The invention belongs to the technical field of preparation methods of chemical products, in particular to a preparation method of di-tert-butyl dicarbonate. Background technique [0002] The molecular formula of di-tert-butyl dicarbonate is C 10 h 9 o 5 , the molecular weight is 209, and the structural formula is: [0003] [0004] The physical and chemical properties of di-tert-butyl dicarbonate are white crystalline or colorless transparent liquid with special odor. Soluble in benzene solvents, soluble in petroleum ether, ethyl acetate and other organic solvents, insoluble in water. It is mainly used as a protective agent for the production of amino acids, as well as the synthesis of medicines and pesticides. [0005] The existing preparation methods of di-tert-butyl dicarbonate include: taking metal potassium salt or sodium salt of mono-tert-butyl carbonate as raw material, reacting with aromatic or aliphatic sulfonyl chloride to generate d...

Claims

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Application Information

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IPC IPC(8): C07C69/96C07C68/02
Inventor 荆和祥王海峻王光权韦中华
Owner 宁夏金象医药化工有限公司
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