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Method for high pressure hydrogenation preparation of L-prolinol from L-proline

A high-pressure hydrogenation and proline technology, applied in organic chemistry and other fields, can solve the problems of long process route, large pollution, troublesome post-processing, etc., and achieve high yield, short process route, and simple post-processing effect

Inactive Publication Date: 2015-08-12
吴志明
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] This process is a commonly used process at present. Compared with direct reduction, the yield is about 80%, but it also has the disadvantages of troublesome post-processing, long process route, large pollution, and is not suitable for large-scale production.

Method used

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  • Method for high pressure hydrogenation preparation of L-prolinol from L-proline
  • Method for high pressure hydrogenation preparation of L-prolinol from L-proline
  • Method for high pressure hydrogenation preparation of L-prolinol from L-proline

Examples

Experimental program
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Effect test

Embodiment 1

[0026] L-proline 10g, solvent isopropanol 20g, catalyst 5% Ru / C (self-made 50% moisture) 1g, phosphoric acid 0.1g, control pressure at 6-8MPa, temperature 140-150°C, reduce for 8h to obtain L - prolinol, (sampling analysis GC L-prolinol 95.6%).

Embodiment 2

[0028] 50g of L-proline, 100g of solvent isopropanol, 5g of catalyst 5%Ru / C (50% moisture by self-made), 0.5g of phosphoric acid, controlled pressure at 6-8MPa, temperature 140-150°C, reduced for 8h, obtained L - prolinol, (sampling analysis GC L-prolinol 95.9%).

Embodiment 3

[0030] L-proline 100g, solvent isopropanol 200g, catalyst 5%Ru / C (self-made 50% moisture) 10g, phosphoric acid 1g, control pressure at 6-8MPa, temperature 140-150°C, reduce for 8h to obtain L-proline Amino alcohol, (sampling analysis GC L-prolinol 95.7%), add sodium hydroxide 6g, after filtering out catalyst, reclaim isopropanol, rectification under reduced pressure obtains L-prolinol 80.8g, yield 92%, GC detection content 99.2%.

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Abstract

The invention discloses a method for high pressure hydrogenation preparation of L-prolinol from L-proline. The method comprises that L-proline in a solvent is reduced in the presence of a catalyst and a catalysis acid at a temperature of 120-180 DEG C under reaction pressure of 4-10MPa for 4-12h to produce a desired product L-prolinol, wherein preferably, the solvent is isopropanol, the catalyst is Ru / C with content of 5% and the catalysis acid is phosphoric acid. The method for high pressure hydrogenation preparation of L-prolinol has the advantages of short technology route, high yield and simple and easy post-treatment processes.

Description

technical field [0001] The invention relates to a method for preparing L-prolinol, in particular to a method for preparing L-prolinol by high-pressure hydrogenation of L-proline. Background technique [0002] L-proline is one of the important amino acids for the synthesis of human protein, an important raw material for amino acid infusion, and the main intermediate for the synthesis of first-line antihypertensive drugs such as captopril and enalapril. It has been widely used in food and Pharmaceutical and other industries. Its reduction product L-prolinol is an important chiral chemical reagent, which is not only a raw material for the synthesis of excellent optical materials and chiral polymer materials, but also an important chiral source for the synthesis of chiral drugs. In recent years, with the rapid development of asymmetric catalytic technology, L-prolinol has become an excellent ligand for metal coordination catalysis, and is widely used in asymmetric metal alkylat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/08
CPCC07D207/08
Inventor 吴志明
Owner 吴志明
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