CN1477095A - Production method of N-benzyl glycine ethyl ester - Google Patents
Production method of N-benzyl glycine ethyl ester Download PDFInfo
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- CN1477095A CN1477095A CNA031320163A CN03132016A CN1477095A CN 1477095 A CN1477095 A CN 1477095A CN A031320163 A CNA031320163 A CN A031320163A CN 03132016 A CN03132016 A CN 03132016A CN 1477095 A CN1477095 A CN 1477095A
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- ethyl ester
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- ester according
- benzylglycine ethyl
- benzylglycine
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Abstract
The present invention discloses a production method of N-benzyl glycine ethyl ester. In the presence of catalyst and organic solvent it makes the benzyl chloride and glycine ethyl ester produce reaction to obtain N-benzyl glycine ethyl ester.
Description
Technical field:
The present invention relates to a kind of production method of N-n-benzylglycine ethyl ester.
Background technology:
Generally to adopt phenyl aldehyde, chlorine, glycine ethyl ester be main raw material in the production of N-n-benzylglycine ethyl ester in the prior art, form through three-step reaction, and its reactions steps complexity, the manufacturing cost height, product content is lower.
Summary of the invention:
The object of the present invention is to provide a kind of step simple, the production method of easy-operating N-n-benzylglycine ethyl ester.
Technical solution of the present invention is:
A kind of production method of N-n-benzylglycine ethyl ester, its feature: under the condition that catalyzer, organic solvent exist, reaction generates the N-n-benzylglycine ethyl ester with benzyl chlorine, glycine ethyl ester:
Above-mentioned catalyzer is the mixture of pyridine and xylidene(s).
The weight ratio of pyridine and xylidene(s) is 1～5 in the catalyzer: 1.
Organic solvent is toluene or o-Xylol, p-Xylol, m-xylene.
The weight ratio of each component consumption is in the reaction system:
Benzyl chlorine: glycine ethyl ester=1: 1.5～3, catalyst consumption are 5～10% of benzyl chlorine consumptions, and solvent load is 4～10 times of glycine ethyl ester.
Temperature of reaction is 110～140 ℃.Reaction times is 6～12 hours.During reaction, also be added with anhydrous sodium sulphate, its consumption is 30～150% of benzyl chlorine consumption by weight.
After reaction is finished, also product is separated purification.
Separating purification step is: will filter through reacted reaction system, and get filtrate, and the filtrate distillation be handled again, will distill substrate then and carry out rectification process, and collect cut, and get product.The temperature that distillation is handled is 105～115 ℃.The temperature of rectification process is that 142～143 ℃, pressure are 10mmHg.
Technology of the present invention is simple, reactions steps is few, and is easy to operate, and production cost is low, the product yield height.
The invention will be further described below in conjunction with embodiment.
Embodiment:
Embodiment 1:
A kind of production method of N-n-benzylglycine ethyl ester, benzyl chlorine, glycine ethyl ester are reacted under the condition that catalyzer, organic solvent exist, also be added with anhydrous sodium sulphate in the reaction system, temperature of reaction is 110～140 ℃, reacted 6～12 hours, and generated the N-n-benzylglycine ethyl ester:
Above-mentioned catalyzer is the mixture of pyridine and xylidene(s), and the weight ratio of pyridine and xylidene(s) is 1～5: 1 (example 1: 1,3: 1,5: 1).Organic solvent is toluene (or o-Xylol, p-Xylol, m-xylene).The weight ratio of each component consumption is in the reaction system: benzyl chlorine: glycine ethyl ester=1: 1.5～3 (example 1: 1.5,1: 2,1: 3), catalyst consumption is 5～10% (examples 5%, 8%, 10%) of benzyl chlorine consumption, solvent load is 4～10 times (4,6,8,10 times of examples) of glycine ethyl ester, and the consumption of anhydrous sodium sulphate is 30～150% (examples 30%, 80%, 110%, 150%) of benzyl chlorine consumption by weight.
After reaction is finished, reaction system is filtered, get filtrate, again filtrate is distilled down 110～125 ℃ (can be 110 ℃, 118 ℃, 125 ℃) and handle, to distill substrate then and carry out rectification process, collect the cut under 142～143 ℃, 10mmHg, product, product content reaches more than 97.0%.
Claims (10)
1, a kind of production method of N-n-benzylglycine ethyl ester is characterized in that: under the condition that catalyzer, organic solvent exist, reaction generates the N-n-benzylglycine ethyl ester with benzyl chlorine, glycine ethyl ester:
Above-mentioned catalyzer is the mixture of pyridine and xylidene(s).
2, the production method of N-n-benzylglycine ethyl ester according to claim 1 is characterized in that: the weight ratio of pyridine and xylidene(s) is 1～5 in the catalyzer: 1.
3, the production method of N-n-benzylglycine ethyl ester according to claim 1 and 2 is characterized in that: organic solvent is toluene or o-Xylol, p-Xylol, m-xylene.
4, the production method of N-n-benzylglycine ethyl ester according to claim 1 and 2 is characterized in that: the weight ratio of each component consumption is in the reaction system:
Benzyl chlorine: glycine ethyl ester=1: 1.5～3, catalyst consumption are 5～10% of benzyl chlorine consumptions, and solvent load is 4～10 times of glycine ethyl ester.
5, the production method of N-n-benzylglycine ethyl ester according to claim 1 and 2 is characterized in that: during reaction, also be added with anhydrous sodium sulphate, its consumption is 30～150% of benzyl chlorine consumption by weight.
6, the production method of N-n-benzylglycine ethyl ester according to claim 1 and 2 is characterized in that: temperature of reaction is 110～140 ℃.
7, the production method of N-n-benzylglycine ethyl ester according to claim 1 and 2 is characterized in that: after reaction is finished, also product is separated purification.
8, the production method of N-n-benzylglycine ethyl ester according to claim 7 is characterized in that: separating purification step is: will filter through reacted reaction system, and get filtrate, again the filtrate distillation is handled, to distill substrate then and carry out rectification process, collect cut, get product.
9, the production method of N-n-benzylglycine ethyl ester according to claim 8 is characterized in that: the temperature that distillation is handled is 105～115 ℃.
10, the production method of N-n-benzylglycine ethyl ester according to claim 8 is characterized in that: the temperature of rectification process is that 142～143 ℃, pressure are 10mmHg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03132016 CN1202076C (en) | 2003-07-08 | 2003-07-08 | Production method of N-benzyl glycine ethyl ester |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03132016 CN1202076C (en) | 2003-07-08 | 2003-07-08 | Production method of N-benzyl glycine ethyl ester |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1477095A true CN1477095A (en) | 2004-02-25 |
| CN1202076C CN1202076C (en) | 2005-05-18 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03132016 Expired - Lifetime CN1202076C (en) | 2003-07-08 | 2003-07-08 | Production method of N-benzyl glycine ethyl ester |
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| CN (1) | CN1202076C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105906819A (en) * | 2016-06-15 | 2016-08-31 | 郑州轻工业学院 | Preparation method of N-benzylglycine ethyl ester small organic molecule gel and application thereof |
-
2003
- 2003-07-08 CN CN 03132016 patent/CN1202076C/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105906819A (en) * | 2016-06-15 | 2016-08-31 | 郑州轻工业学院 | Preparation method of N-benzylglycine ethyl ester small organic molecule gel and application thereof |
| CN105906819B (en) * | 2016-06-15 | 2018-09-28 | 郑州轻工业学院 | A kind of preparation method and applications of N- benzyl glycines ester Low Molecular-Weight Gel |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1202076C (en) | 2005-05-18 |
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Address after: 226401 Jiangsu province Rudong Matang town Jianshe Road County No. 40 -1 Patentee after: JIANGSU U-PREFER BIOCHEMICAL TECHNOLOGY CO.,LTD. Address before: 226401 Jiangsu province Rudong Matang town Jianshe Road County No. 40 -1 Patentee before: Nantong Dongchang Chemical Industrial Co.,Ltd. |
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Granted publication date: 20050518 |