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Preparing technology of D-galactosamine hydrochloride

A technology for lactosamine hydrochloride and preparation process, which is applied in the field of preparation technology of D-galactosamine hydrochloride, can solve the problems of low yield and low yield, and achieves improved reaction process, stable product quality, and improved operation. cumbersome effect

Inactive Publication Date: 2019-08-23
南京博源医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The above-mentioned existing technical solutions have the following defects: the above-mentioned preparation method obtains D-galactosamine hydrochloride, the weight yield is only 25%, the yield is low, and the yield is low. This problem needs to be solved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The invention discloses a preparation process of D-galactosamine hydrochloride. Add 500ml of absolute ethanol into a 1000ml three-necked flask equipped with a reflux condenser, a stirrer and a thermometer, stir at room temperature and add 100g of di Methyldodecylamine, 500g of solid-phase silica, heated to 110°C within 30 minutes, maintained at reflux for 5 hours and then lowered to 29°C, filtered and dried to obtain 589g of organic amine immobilized catalyst.

[0021] Add 190g of 5-methyltryptamine hydrochloride and 600ml of dimethylamide respectively in a 1000ml three-necked flask with a stirrer and a thermometer, add 59g of organic amine immobilized catalyst and 150g of chloropropene, and react for eight hours at room temperature. Liquid was filtered, the obtained filtrate was evaporated to dryness, dissolved in 1150ml of isopropanol, and 89ml of 36wt% hydrochloric acid was added for hydrochloric acidification to obtain 130.32g of white crystals of D-galactosamine hyd...

Embodiment 2

[0023] The invention discloses a preparation process of D-galactosamine hydrochloride. Add 500ml of absolute ethanol into a 1000ml three-necked flask equipped with a reflux condenser, a stirrer and a thermometer, stir at room temperature and add 100g of di Methyldodecylamine, 500g of solid-phase silica, heated to 110°C within 30 minutes, maintained at reflux for 5 hours, then lowered to 29°C, filtered and dried to obtain 589g of organic amine immobilized catalyst.

[0024] Add 190g of 5-methyltryptamine hydrochloride and 800ml of dimethylamide respectively in a 1000ml three-necked flask with a stirrer and a thermometer, add 104g of organic amine immobilized catalyst and 200g of chloropropene, and react for six hours at room temperature. Liquid was filtered, the obtained filtrate was evaporated to dryness, dissolved in 1654ml of isopropanol, added 100ml of 36wt% hydrochloric acid for hydrochloric acidification, and 141.05g of white crystals of D-galactosamine hydrochloride were ...

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Abstract

The invention discloses a preparing technology of D-galactosamine hydrochloride, and relates to the technical field of intermediates of anti-hepatopathy drugs. The preparing technology aims at solvingthe problem in the prior art that the weight yield of the D-galactosamine hydrochloride is only 25%, and the yield is low. The preparing technology is characterized in that 5-methyltryptamine hydrochloride is dissolved in dimethylformamide, an organic amine immobilized catalyst and chloropropene are added, a reaction is carried out for 5-6 hours at normal temperature, a filtrate obtained after filtering of a reaction liquid is dried by distillation, afterwards, isopropanol is adopted for dissolution, 34 wt% hydrochloric acid is added for hydrochlorination, and then the target product is obtained. Preparation of the organic amine immobilized catalyst comprises the following steps of adding organic amine and an immobilization phase into absolute ethyl alcohol, conducting backflow, cooling,filtering and drying, and then obtaining the organic amine immobilized catalyst, wherein the organic amine is dodecyl-tetradecyl dimethyl amine, and the immobilization phase is silicon oxide. By meansof the preparing method, the effect of increasing the production yield of the D-galactosamine hydrochloride is achieved.

Description

technical field [0001] The invention relates to the technical field of anti-hepatopathy drug intermediates, in particular to a preparation process of D-galactosamine hydrochloride. Background technique [0002] D-galactosamine hydrochloride is a nucleoside metabolism disruptor in liver cells, which can continuously damage liver cells. It is mainly used for liver pathology and biochemical research. The hepatitis model replicated with it is close to the pathological changes of human hepatitis. It is suitable for screening And research on anti-hepatitis drugs is more reliable and useful. [0003] The existing Chinese patent with publication number CN1036386A discloses a preparation method of D-galactosamine hydrochloride, which uses chondroitin sulfate as raw material and prepares D-galactosamine hydrochloride through hydrolysis with hydrochloric acid, which is characterized in that chondroitin sulfate The crude element does not need to be pretreated, it is directly hydrolyzed...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H5/06C07H1/00B01J31/02
CPCC07H5/06C07H1/00B01J31/0239
Inventor 陈建国张国品
Owner 南京博源医药科技有限公司