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Preparation method of cis-3-amino-cyclopentanol hydrochloride

A technology of cyclopentanol hydrochloride and cyclopentanol, which is applied in the preparation of aminohydroxy compounds, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problem of low purity of cis-3-amino-cyclopentanol and potential explosion The problems of danger and low industrialization methods can reduce the difficulty of purification, improve the yield, and the process is simple and convenient.

Inactive Publication Date: 2014-05-14
甘肃科瑞生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The means of industrialization are very low, the use of highly toxic reagents and the potential danger of explosion, and the production process is backward
Cause the productive rate of this synthesis process to be low, the purity of the synthesized cis-3-amino-cyclopentanol is low, the purification is complicated, the energy consumption is large, the raw material cost is too high, and the pollution is more serious

Method used

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  • Preparation method of cis-3-amino-cyclopentanol hydrochloride
  • Preparation method of cis-3-amino-cyclopentanol hydrochloride

Examples

Experimental program
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Effect test

Embodiment 1

[0031] According to the molar ratio of 1:2, take benzyloxycarbonyl chloride and hydroxylamine hydrochloride respectively, dissolve them in dichloromethane, react at room temperature for 16 hours, purify the reaction product, wash the organic phase with saturated brine, and dry, at 30℃~40℃ Remove dichloromethane at temperature and recrystallize to obtain cis 3-amino-cyclopentanol intermediate A; molar ratio of 3:1, respectively take redistilled cyclopentadiene and cis 3-amino prepared in step 1. -Cyclopentanol Intermediate A, dissolved in dichloromethane, add sodium periodate and tetrabutylammonium bromide to react for 6 hours at a temperature of 0℃~5℃, and purify the product to obtain cis-3 -Amino-cyclopentanol intermediate B; Take the catalyst and cis 3-amino-cyclopentanol intermediate B at a molar ratio of 0.1:1, dissolve them in methanol, blow hydrogen gas to 50Psi at room temperature, react for 10 hours, and purify to produce Material, the system of crude cis 3-amino-cyclop...

Embodiment 2

[0038] According to the molar ratio of 1:2.5, take benzyloxycarbonyl chloride and hydroxylamine hydrochloride respectively, dissolve them in dichloromethane, react for 10 hours at room temperature, purify the reaction product, wash the organic phase with saturated brine, and dry it at 30℃~40℃ Remove dichloromethane at temperature and recrystallize to obtain cis 3-amino-cyclopentanol intermediate A; molar ratio of 2.2:1, respectively take redistilled cyclopentadiene and cis 3-amino prepared in step 1 -Cyclopentanol intermediate A, dissolved in dichloromethane, add sodium periodate and tetrabutylammonium bromide to react for 4 hours at a temperature of 0°C to 5°C, and purify the product to obtain cis-3 -Amino-cyclopentanol intermediate B; According to the molar ratio of 0.05:1, take the catalyst and the cis 3-amino-cyclopentanol intermediate B respectively, dissolve them in methanol, blow hydrogen gas to 50Psi at room temperature, react for 10 hours, and purify to produce Materia...

Embodiment 3

[0041] According to the molar ratio of 1:2.5, take benzyloxycarbonyl chloride and hydroxylamine hydrochloride respectively, dissolve them in dichloromethane, react for 16 hours at room temperature, purify the reaction product, wash the organic phase with saturated brine, and dry, at 30℃~40℃ Remove dichloromethane at temperature, recrystallize to obtain cis 3-amino-cyclopentanol intermediate A; molar ratio 4:1, take re-distilled cyclopentadiene and cis 3-amino prepared in step 1 respectively -Cyclopentanol Intermediate A, dissolved in dichloromethane, add sodium periodate and tetrabutylammonium bromide to react for 6 hours at a temperature of 0°C to 5°C, and purify the product to obtain cis-3 -Amino-cyclopentanol intermediate B; Take the catalyst and cis 3-amino-cyclopentanol intermediate B at a molar ratio of 0.1:1, dissolve them in methanol, blow hydrogen gas to 50Psi at room temperature, react for 10 hours, and purify to produce Material, the system of crude cis 3-amino-cyclo...

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Abstract

The invention discloses a preparation method of cis-3-amino-cyclopentanol hydrochloride, which comprises the steps of: (1) preparing a cis-3-amino-cyclopentanol intermediate A; (2) preparing a cis-3-amino-cyclopentanol intermediate B; (3) preparing a cis-3-amino-cyclopentanol crude product; (4) preparing a cis-3-amino-cyclopentanol hydrochloride crude product; and (5) obtaining the final product. The preparation method of the cis-3-amino-cyclopentanol hydrochloride has the advantages of being high in yield and purity, low in cost, safe and free from pollution.

Description

technical field [0001] The invention relates to a method for preparing a compound, in particular to a method for preparing cis-3-amino-cyclopentanol hydrochloride. Background technique [0002] cis-3-amino-cyclopentanol hydrochloride is a very important intermediate of pharmaceuticals and other chemical additives. The annual international demand is about 10 tons. Most of them are manufactured by foreign manufacturers, and there is no domestic production. mass-produced companies. At present, the process of synthesizing cis-3-amino-cyclopentanol hydrochloride is to use 2-cyclopentenone as raw material, dichloromethane as solvent, acetic acid, sodium azide or azidotrimethylsilane for reaction, hydrogenation Reduction followed by sodium borohydride reduction affords the product. The means of industrialization are very low, the use of highly toxic reagents and the potential danger of explosion, and the production process is backward. As a result, the yield of the synthesis pro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C215/20C07C213/08
Inventor 张泰
Owner 甘肃科瑞生物科技有限公司
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