Preparation of lactitol

A technology for lactitol and aqueous solution, which is applied in the field of synthesis of lactitol, can solve the problems of inability to prepare crystalline lactitol monohydrate, difficult control of reaction degree, unstable product quality, etc., and achieve low production cost, Simplified operation and good product quality

Active Publication Date: 2009-07-15
YANGTZE RIVER PHARM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] For the synthesis of lactitol, as early as 1920, Senderens first used Raney Ni as a catalyst to catalytic hydrogenation to prepare lactitol syrup, and further synthesized crystalline lactitol, called lactitol monohydrate, with a melting point of 78°C; In 1938, Wolfom also used Raney Ni as a catalyst to prepare lactitol syrup through high-pressure catalytic hydrogenation at a high temperature of 145°C and 138 atmospheres. After one month of crystallization, anhydrous crystals of lactitol were obtained, but the product was very easy to absorb. In 1952, Wolform made a process improvement and synthesized the dihydrate of lactitol, which confirmed that the melting point of the dihydrate was 72.5-74 ° C, thus overturning the lactitol synthesized by Senderens as a monohydrate; In 1978, Saijonmaa further improved the catalytic hydrogenation process of Raney Ni as a catalyst. The lactose solution was 30% (W / V), and the amount of Raney Ni was reacted at 100°C under 86.5 atmospheres to prepare a 97% milk The syrup of pitol, although temperature and pressure have all reduced, it can only be prepared the transparent syrup of high concentration, but can't prepare crystalline lactitol monohydrate, and the lactitol prepared under high temperature and pressure is violently poor again. To foreign matter into lactulose, the reaction conditions are harsh, the degree of reaction is not easy to control, and the quality of the product is unstable

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0012] Weigh 54g of lactose and dissolve it in 450ml of water, cool to -10~10°C, add 80ml of potassium borohydride solution dropwise, stir and react at 10°C for 1h, and continue stirring at 35°C for 6h. Add 80ml of acidic cationic resin to neutralize until no gas is released, stir, filter, and wash three times, treat the cationic resin with 1N_HCl, regenerate and recover, add 80ml of anionic resin to the mother liquor, stir, filter, drain, wash three times with 50ml of purified water, and depressurize Concentrate to obtain the transparent syrup of lactitol.

[0013] Take 43g of the transparent syrup obtained above and heat it to 100°C, then slowly cool it down, add 4 times the amount of ethanol, stir, add seed crystals, and then slowly precipitate. After 24 hours, white crystals precipitate, drain, dry, and collect Rate 60%.

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PUM

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Abstract

The invention discloses a preparation method of synthesizing lactitol with lactose as a starting material. In the method, lactose is taken as the starting material to synthesize the lactitol by one step. The preparation method comprises the following steps: taking potassium borohydride as a reducing agent and reacting at a suitable temperature to avoid a high-temperature and high-pressure reaction required before, and hydrolyzing with cation exchange resin and removing impurities with anion exchange resin during the reaction, thus obtaining the lactitol. On the basis of the prior art, the preparation method simplifies operation, overcomes the disadvantages of high-temperature and high-pressure strict reaction conditions required before, hard control on extent of reaction, and has the advantages of simple operation, high safety, good product quality, low cost and the like.

Description

technical field [0001] The invention relates to the field of pharmaceutical synthesis, in particular to a preparation method for synthesizing lactitol with lactose as a starting material. Background technique [0002] Lactitol, also known as lactitol monohydrate, has a chemical name of 4-0-β-D-galactopyranosyl-D-sorbitol monohydrate. Lactitol can effectively treat hepatic portal encephalopathy. It cannot be decomposed and absorbed in the small intestine and enters the colon in its original form. In the colon, it is degraded by Bacteroides and Lactobacillus in the intestinal microorganisms, and acetic acid is generated during the process. acid and butyrate, thereby acidifying the contents of the colon and reducing the absorption of ammonia by the colon. [0003] For the synthesis of lactitol, as early as 1920, Senderens first used Raney Ni as a catalyst to catalytic hydrogenation to prepare lactitol syrup, and further synthesized crystalline lactitol, called lactitol monohyd...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): C07H15/04A61P25/00A61P43/00
Inventor孙田江杨俊陆宏国赵文镜冯建鹏高力虎朱年青张虎跃霍浩刚张玉斌
OwnerYANGTZE RIVER PHARM GRP CO LTD