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Preparation method of CBZ-L-valine

A technology of CBZ-L- and valine, applied in the preparation of carbamic acid derivatives, preparation of organic compounds, organic chemical methods, etc., can solve the problems of lowering the quality of final products, inconvenient temperature control, and poor practicability, etc. Achieve the effects of simple structure, increased production quality, and strong practicability

Pending Publication Date: 2020-12-01
ZHEJIANG TIANRUI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, the preparation method of CBZ-L-valine on the market is not convenient for temperature control because of the large temperature difference required, resulting in reduced quality of the final product, poor practicability, and how to ensure the temperature control Controlling accuracy and ensuring the stability of the reaction environment are also current problems

Method used

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  • Preparation method of CBZ-L-valine
  • Preparation method of CBZ-L-valine

Examples

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Embodiment Construction

[0024] refer to Figure 1 to Figure 2 A preparation method example of CBZ-L-valine of the present invention will be further described.

[0025] For ease of description, if spatially relative terms such as "upper", "lower", "left", and "right" are used in the embodiments, they are used to describe the relative relationship between one element or feature shown in the figure and another element or feature Relationship. It will be understood that the spatial terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures. For example, if the device in the figures is turned over, elements described as "below" other elements or features would then be oriented "above" the other elements or features. Thus, the exemplary term "lower" can encompass both an orientation of above and below. The device may be otherwise oriented (rotated 90 degrees or at other orientations) and the spatially relative specifica...

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Abstract

The invention discloses a preparation method of CBZ-L-valine. The invention aims to provide the preparation method of CBZ-L-valine, with the advantages of good reaction effect, high temperature control precision and high practicality. The preparation method is characterized by comprising the following steps: (1) taking and adding 11.7 Kg of 10mol / L L-valine, 50 L of a 2 mol / L sodium hydroxide solution and a 10 mol / L sodium carbonate into a 200 L reaction kettle, and starting stirring until the L-valine is dissolved; (2) after the L-valine is completely dissolved, reducing the temperature of the solution to 0 DEG C or below, dropwise adding 50 L of a 1, 4-dioxane solution containing 20.5 Kg of benzyl chloroformate, keeping the temperature of the solution between 10 DEG C and 20 DEG C in thedrop-by-drop adding process, and reacting for 8 h at room temperature after drop-by-drop adding is finished; and (3) fully stirring the mixed solution obtained in step (2) until no obvious reactant is generated, extracting the reaction solution with 25 L of dichloromethane, discarding the obtained organic phase, cooling the obtained water phase to 10 DEG C or below, dropwise adding concentrated hydrochloric acid until the pH value is equal to 2, stirring at 10 DEG C or below for 60-80 minutes to separate out a large amount of white solid, carrying out suction filtration, and washing the filter residue with water. The method is suitable for the technical field of preparation of CBZ-L-valine.

Description

technical field [0001] The present invention relates to a kind of technical field of CBZ-L-valine preparation, more specifically, it relates to a kind of preparation method of CBZ-L-valine. Background technique [0002] At present, the preparation method of CBZ-L-valine on the market is not convenient for temperature control because of the large temperature difference required, resulting in reduced quality of the final product, poor practicability, and how to ensure the temperature control Controlling accuracy and ensuring the stability of the reaction environment are also current problems. Contents of the invention [0003] Aiming at the deficiencies in the prior art, the object of the present invention is to provide a CBZ-L-valine preparation method with good reaction effect, high temperature control precision and strong practicability. [0004] In order to achieve the above object, the present invention provides the following technical scheme: a kind of preparation met...

Claims

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Application Information

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IPC IPC(8): C07C269/04C07C269/08C07C271/22G05D27/02
CPCC07C269/04C07C269/08G05D27/02C07B2200/07C07C271/22
Inventor 张胜
Owner ZHEJIANG TIANRUI CHEM
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