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Synthesizing method of drug intermediate 5-chloro-2-pentanone

A synthesis method and intermediate technology, which are applied in the synthesis field of 5-chloro-2-pentanone, can solve the problems of harsh reaction conditions, many processes, difficult control and the like, and achieve the effect of good stability

Inactive Publication Date: 2015-03-25
SUZHOU JONATHAN NEW MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the production raw materials involved in the synthesis are expensive and difficult to obtain. If it is applied to industrial production, it will not produce corresponding economic benefits, so it will not be widely used.
In some methods for synthesizing 5-chloro-2-pentanone, although the raw materials are high, the egg process is complicated, the process is too many, it is not easy to control, and it is difficult to apply it to a large amount of industrial production.
There are also methods involving precious metal catalysts, which are not only expensive, but also have extremely strict requirements on reaction conditions. Once the control is not done properly, it will cause inestimable losses.

Method used

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  • Synthesizing method of drug intermediate 5-chloro-2-pentanone
  • Synthesizing method of drug intermediate 5-chloro-2-pentanone

Examples

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Embodiment Construction

[0007] The following will be described in conjunction with specific embodiments.

[0008] The 3-acetyl n-propanol used in this example is industrial grade, with a density of 1.0071, a purity of >99%, and a boiling point of 208°C. Hydrochloric acid pseudo-industrial grade, with a purity of 31%-32%, configured to a concentration of 21%. The reaction was carried out under the conditions of temperature T=100°C, vacuum degree P=-0.045MPa, and the molar ratio of 3-acetyl n-propanol to HCl was N=1:2. The moles of 3-acetyl n-propanol were 0.2mol, 0.4mol, 0.6mol, 0.8mol, 1.2mol, and 1.4mol respectively, and the reaction was carried out, and the peak appeared in 7.9 minutes, and the reaction was completed in 12 minutes. The results are shown in the table below:

[0009]

[0010]

[0011] It can be seen from the above table that the method has good stability, the yield is basically the same, the repeatability error is less than 1%, and the moisture content is less than 5%. The m...

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Abstract

The invention discloses a synthesizing method of drug intermediate 5-chloro-2-pentanone. 3-acetyl-1-propanol and HCl are used as raw materials and have a chemical reaction under conditions as follows: the temperature T is 100 DEG C, the vacuum degree P is minus 0.045 MPa, the mole ratio N of the 3-acetyl-1-propanol to the HCl is 1:2, and the concentration of the HCl is 21%. With the adoption of the method, the conditions of the temperature, the vacuum degree, the mole ratio of the raw materials and the concentration of the raw materials for synthesis of the 5-chloro-2-pentanone are optimized, the mole yield of the 5-chloro-2-pentanone reaches 92% under industrial conditions, and the stability is good.

Description

technical field [0001] The invention belongs to the field of medicine and relates to a synthesis method of a drug intermediate, in particular to a synthesis method of 5-chloro-2-pentanone. Background technique [0002] 5-Chloro-2-pentanone is the starting material for the synthesis of various chemical drugs, such as chloroquine phosphate hydrochloride, 5-diethylamino-2-pentanone, or indirectly cooperate with ciprofloxacin and quinolones drug. In the prior art, the synthesis method of 5-chloro-2-pentanone is simple, the synthesis conditions are mild, and it is relatively suitable for large-scale production. However, the production raw materials involved in the synthesis are expensive and difficult to obtain. If it is applied to actual industrial production, it will not produce corresponding economic benefits, so it will not be widely used. In some methods for synthesizing 5-chloro-2-pentanone, although the raw materials are high, the egg process is complicated, the process ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/63C07C49/16
CPCC07C45/63C07C49/16
Inventor 李卓才李苏杨
Owner SUZHOU JONATHAN NEW MATERIALS TECH