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Preparation method of N-benzyloxycarbonyl-L-norleucine

A technology of benzyloxycarbonyl and hexanine, which is applied in the preparation of carbamic acid derivatives, organic compounds, chemical instruments and methods, etc., can solve the problems of low purity, cumbersome synthesis process, and high cost, so as to improve the purity, The effect of simple process and low cost

Inactive Publication Date: 2019-08-20
南京博源医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] N-benzyloxycarbonyl-L-hexanine is a relatively common pharmaceutical intermediate, which is used in pharmaceutical synthesis. The existing synthesis process of N-benzyloxycarbonyl-L-hexanine is cumbersome, with high cost and low purity. , for this reason, the present invention proposes a kind of preparation method of N-benzyloxycarbonyl-L-hexanoic acid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A kind of preparation method of N-benzyloxycarbonyl-L-hexanoic acid that the present invention proposes, comprises the following steps,

[0018] S1, adding L-hexanoic acid and alkali to the organic solvent, the weight of the organic solvent is 6 times of the weight of L-hexanoic acid;

[0019] S2, add benzyl chloroformate dropwise to the solution of S1, react at 25°C for 2.5 hours after the drop, heat to reflux after the reaction, separate the water generated by the reaction with a water separator, cool down to 10°C, and obtain N - Benzyloxycarbonyl-L-hexanoic acid feed solution;

[0020] S3, further purification: put the N-benzyloxycarbonyl-L-hexanine feed solution into a centrifuge, adjust the rotating speed of the centrifuge to 10000r / min, and then centrifuge for 2min to obtain the separated centrifugal liquid, and put the upper part of the centrifugal liquid The supernatant liquid is discharged, and the remaining part of the N-benzyloxycarbonyl-L-hexanine solution ...

Embodiment 2

[0022] A kind of preparation method of N-benzyloxycarbonyl-L-hexanoic acid that the present invention proposes, comprises the following steps,

[0023] S1, adding L-hexanoic acid and alkali to the organic solvent, the weight of the organic solvent is 7 times of the weight of L-hexanoic acid;

[0024] S2, add benzyl chloroformate dropwise to the solution of S1, react at 30°C for 3.2 hours after the drop, heat to reflux after the reaction, separate the water generated by the reaction with a water separator, cool down to 12°C, and obtain N - Benzyloxycarbonyl-L-hexanoic acid feed solution;

[0025] S3, further purification: put the N-benzyloxycarbonyl-L-hexanine feed solution into a centrifuge, adjust the rotating speed of the centrifuge to 11000r / min, and then centrifuge for 3min to obtain the divided centrifuged liquid. The supernatant liquid is discharged, and the remaining part of the N-benzyloxycarbonyl-L-hexanine solution is the N-benzyloxycarbonyl-L-hexanine that needs to...

Embodiment 3

[0027] A kind of preparation method of N-benzyloxycarbonyl-L-hexanoic acid that the present invention proposes, comprises the following steps,

[0028] S1, adding L-hexanoic acid and alkali to the organic solvent, the weight of the organic solvent is 8 times of the weight of L-hexanoic acid;

[0029] S2, add benzyl chloroformate dropwise to the solution of S1, react at 35°C for 4.5 hours after the drop, heat to reflux after the reaction, separate the water generated by the reaction with a water separator, cool down to 15°C, and obtain N - Benzyloxycarbonyl-L-hexanoic acid feed solution;

[0030] S3, further purification: put the N-benzyloxycarbonyl-L-hexanine feed liquid into a centrifuge, adjust the rotating speed of the centrifuge to 12000r / min, and then centrifuge for 4min to obtain the divided centrifuged liquid. The supernatant liquid is discharged, and the remaining part of the N-benzyloxycarbonyl-L-hexanine solution is the N-benzyloxycarbonyl-L-hexanine that needs to b...

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Abstract

The invention discloses a preparation method of N-benzyloxycarbonyl-L-norleucine, and belongs to the field of medicine intermediates. The method comprises the following steps: S1, adding L-norleucineand an alkali to an organic solvent, wherein the weight of the organic solvent is 6-8 times the weight of the L-norleucine; S2, adding benzyl chloroformate to a solution obtained in step S1, separating water, generated through a reaction, by a water separator, and cooling the obtained solution to 10-15 DEG C to obtain an N-benzyloxycarbonyl-L-norleucine feed liquid; and S3, further purifying: adding the N-benzyloxycarbonyl-L-norleucine feed liquid into a centrifuge, adjusting the rotating speed of the centrifuge to 10000-12000 r / min, centrifuging the feed liquid for 2-4 min to obtain a layeredcentrifuged liquid, discharging the supernatant of the centrifuged liquid, and reserving the lower N-benzyloxycarbonyl-L-norleucine solution to obtain the required N-benzyloxycarbonyl-L-norleucine. The method has the advantages of simple process, low cost, high purity of the obtained product, and suitableness for being promoted and used.

Description

technical field [0001] The invention relates to the technical field of pharmaceutical intermediates, in particular to a preparation method of N-benzyloxycarbonyl-L-hexanoic acid. Background technique [0002] The so-called pharmaceutical intermediates are actually some chemical raw materials or chemical products used in the process of pharmaceutical synthesis. This kind of chemical product does not require a drug production license, and can be produced in ordinary chemical factories. As long as it reaches a certain level, it can be used in the synthesis of drugs. [0003] N-benzyloxycarbonyl-L-hexanine is a relatively common pharmaceutical intermediate, which is used in pharmaceutical synthesis. The existing synthesis process of N-benzyloxycarbonyl-L-hexanine is cumbersome, with high cost and low purity. , For this reason, the present invention proposes a kind of preparation method of N-benzyloxycarbonyl-L-hexanoic acid. Contents of the invention [0004] The purpose of ...

Claims

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Application Information

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IPC IPC(8): C07C269/04C07C271/22
CPCC07C269/04C07C271/22
Inventor 陈建国袁新辉
Owner 南京博源医药科技有限公司
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