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Method for synthesizing high purity dextrose octylame

A synthesis method and technology of meglucanamine, applied in the direction of oligosaccharides, etc., can solve the problems of increasing reaction time, no industrialization value, and high cost, and achieve the effect of saving cost.

Inactive Publication Date: 2004-06-02
中国科学院成都有机化学研究所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 1972, Perey G.Holton proposed a process of catalytic hydrogenation of Schiff base to prepare octylamine using Raney nickel as a catalyst, but the yield was very low, only 20-40%, and had no industrial value
In 1985, Zhang Linze and others in my country improved the Holton process by increasing the amount of catalyst and increasing the reaction time. The reported yield reached 60%, but the cost was relatively high
In 1988, Li Xuebing of Tsinghua University and others used Raney nickel as a catalyst to form a Schiff base from n-octylamine and then catalyzed hydrogenation to synthesize octylglucosamine. They reported that by adding triethylamine to the reaction system, the activity of the catalyst was improved, and the reaction yield reached 71.4%, but no reports of product purity
In addition, the existing process uses methanol as a detergent, which is highly toxic and has poor washing effect

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0021] 1. Preparation of catalyst

[0022] Dissolve 30g of NaOH in 120ml of water, cool to zero in an ice-water bath, slowly add 30g of aluminum-nickel alloy under electric stirring, react for 2-3 hours below 25 degrees Celsius, continue stirring for 0.5 hours, place at room temperature for 2-3 hours, and heat up to 95-100 Celsius to continue the reaction for 2-3 hours, wash with water until neutral, and then wash 3 times with ethanol. The prepared RaneyNi was stored under the liquid level of ethanol for future use.

[0023] 2. Preparation of catalyst ZCMT

[0024] 3, the preparation of octylglucamine

[0025] Put n-octylamine, glucose, solvent and catalyst into the high-pressure reaction kettle according to a certain ratio, seal it, pass in hydrogen gas to 1.2-1.4Mpa, heat up to 55-65 degrees Celsius, and react for 2 hours, cool and precipitate white crystals, filter , drying at 70 degrees Celsius for 2 hours to obtain the product. After the reaction is completed, the rea...

Embodiment 1

[0029] Embodiment 1: Reactor: 200 liters

[0030] Feeding amount: n-octylamine 15.0KG

[0031] Glucose 22.0KG

[0032] Catalyst / co-catalyst 1.88KG

[0033] Solvent SOW-4 135.0 liters

[0034] Reaction conditions: Reaction temperature 55°C

[0035] Pressure 1.20Mpa

[0036] Response time 3h

[0037] The product yield is 76%, and the product purity is 99.5%.

Embodiment 2

[0039] Reactor: 1000 liters

[0040] Feeding amount: n-octylamine 70.0KG (imported raw materials)

[0041] Glucose 97.7KG (domestic)

[0042] Catalyst / co-catalyst 8.4KG

[0043] Solvent SOW-4 650.0 liters (domestic)

[0044] Reaction conditions: Reaction temperature 55°C

[0045] Pressure 1.20Mpa

[0046] Response time 3h

[0047] The product yield reaches 76.3%, and the product purity is 99.2%.

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Abstract

The present invention provides the preparation process of gluco-octyl amine. Glucose and n-octyl amine in the molar ratio o 1.05 are reacted to produce Schiff base; co-catalyst / RaneyNi system is added to catalytically hydrogenate Schiff base to produce gluco-octyl amine; and through cooling crystallization, centrifugal separation, washing with mixed solvent containing no methanol and drying, refined gluco-octyl amine with purity up to 99.5 % is obtained with product yield up to 76 %, low cost and no environmental pollution.

Description

technical field [0001] The present invention relates to a kind of synthesis method of chiral drug and pesticide alkaline resolving agent, in particular, the present invention relates to a kind of synthesis method of high-purity octylglumine. Background technique [0002] Glucosylamine is a resolving agent for the resolution of chiral drugs and pesticides such as non-steroidal anti-inflammatory analgesics Naproxen, Ibuprofen and Metalaxyl. For the resolution of the above-mentioned chiral drugs and pesticides, a variety of methods have been explored, including: biological enzyme method, chromatography, induced crystallization method and common crystallization method using alkaline resolving agent. Biological enzymatic method and chromatographic method are subject to condition limitations, and industrial application is limited; induced crystallization method still needs to do a lot of technological condition research; better is the ordinary crystalliz...

Claims

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Application Information

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IPC IPC(8): C07H3/06
Inventor 洪军卢林
Owner 中国科学院成都有机化学研究所