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Preparation method and application of stannous amino acid complex

An amino acid stannous and complex technology, which is applied in the preparation of organic compounds, the preparation of cyanide reactions, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problem of low yield, complicated methods, and inability to carry out large-scale Industrial production and other problems, to achieve the effect of low catalyst dosage, simple process and low production cost

Active Publication Date: 2019-08-02
大连汇鹏达化工有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The present invention is directed at the existing synthesis method of amino acid stannous to be obtained by the direct reaction of stannous salt and amino acid in a solvent, and a large amount of toxic organic solvents are used in the process of applying the method to prepare amino acid stannous, the method is complicated, and the yield is relatively high. low, and can only obtain part of the amino acid and tin complexes, it is only suitable for the research of preparing a small amount of stannous amino acid in the laboratory, and cannot carry out large-scale industrial production. For the above-mentioned shortcomings, a kind of stannous amino acid is provided. new synthetic method

Method used

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  • Preparation method and application of stannous amino acid complex
  • Preparation method and application of stannous amino acid complex
  • Preparation method and application of stannous amino acid complex

Examples

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Embodiment 1

[0033] The synthesis of embodiment 1 catalyst L-tin protophenylalanate

[0034] Add L-phenylalanine (9.9g, 0.06mol) and methanol (40ml) into a 100ml three-neck flask, stir and react in a constant temperature water bath at 60°C for 20min, add triethylamine solution (6.07g, 0.06mol) dropwise, Add dropwise in 30 minutes, L-phenylalanine is all dissolved, then feed nitrogen into the solution for 10min, remove the oxygen in the solution and the reaction flask, and add tin protochloride (SnCl 2 2H 2 (2, 6.78g, 0.03mol) 10ml of methanol solution, after 30 minutes of dropwise addition, react at 60°C for 5 hours, the L-stannous phenylalanine is precipitated in granular form, filtered, and the product is dried in a vacuum oven for 24 hours , to obtain 12.4g, yield 12.4 / 13.38×100%=92.68%. Elemental analysis value (composition C 18 h 20 N 2 o 4 Sn) (%) C: 48.43 (47.23), H: 4.48 (4.42), Sn: 26.46 (26.53), (measured in air).

Embodiment 2

[0035] The synthesis of embodiment 2 catalyst L-stannous leucine

[0036] The experimental procedure was the same as in Example 1, except that L-phenylalanine was replaced with 0.06 mol L-leucine to obtain 10.82 g of stannous L-leucine with a yield of 95.33%. Elemental analysis value (composition C 12 h 24 N 2 o 4 Sn) (%) C: 38.05 (37.93), H: 6.34 (6.21), Sn: 31.22 (30.83), (measured in air).

Embodiment 3

[0037] The synthesis of embodiment 3 catalyst L-stannous isoleucine

[0038] The experimental procedure was the same as that in Example 1, except that L-phenylalanine was replaced with 0.06 mol L-isoleucine to obtain 9.93 g stannous L-isoleucine with a yield of 87.49%. Elemental analysis value (composition C 12 h 24 N 2 o 4 Sn) (%) C: 38.05 (37.81), H: 6.34 (6.26), Sn: 31.22 (29.87), (measured in air).

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Abstract

The invention discloses a preparation method and an application of a stannous amino acid complex. The preparation method of the stannous amino acid complex comprises the steps of allowing triethylamine to react with amino acid in an organic medium to form amino acid salt, allowing amino acid salt and neutral stannous salt ligand to give a complex decomposition reaction, and performing filtration and drying to form the stannous amino acid complex. The stannous amino acid complex is a high-efficiency lactone ring opening polymerization catalyst, and can be used for catalyzing a ring opening polymerization reaction of lactone such as lactide; and particularly, high molecular weight polylactic acid can be obtained for polymerization of L-lactide. The novel synthesis method of the stannous amino acid complex and the stannous amino acid complex as the ring opening polymerization catalyst of lactone such as lactide have very obvious advantages; raw materials are cheap; a synthesis route is simple; a product yield is high; the stannous amino acid complex has very high catalytic activity and higher stereoselectivity; a polyester material with higher molecular weight and lower cytotoxicity can be obtained; and the large-scale industrial production requirements can be met.

Description

technical field [0001] The present invention relates to a new synthesis method of an organometallic compound and its use as a catalyst in the ring-opening polymerization of lactone and lactone, in particular to a new synthesis method of stannous amino acid, and the role of stannous amino acid in catalyzing lactide and lactone Use of ring-opening polymerization of lactones. Background technique [0002] The early method of preparing stannous amino acid is to use DMF as a catalyst to obtain the complex of stannous amino acid by azeotropic water removal with tin or alkyl tin oxide and amino acid in benzene solution. This method uses a large amount of toxic organic Solvent, complex method, low yield, and only part of the amino acid stannous complex can be obtained, which cannot be applied to large-scale production [B.Y.K.HO and J.J.ZUCKERMAN*, Inorganic Chemistry, 1973, (7): 1552-1561]. [0003] In the process of transitioning from an exhausted resource economy to a renewable r...

Claims

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Application Information

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IPC IPC(8): C07C229/76C07C227/16C07D207/16C07D209/20B01J31/22C08G63/85C08G63/08
CPCC07C229/76C07C227/16C07D207/16C07D209/20B01J31/2217C08G63/823B01J2231/14
Inventor 魏志勇贺毛毛孙明臣
Owner 大连汇鹏达化工有限公司
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