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
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[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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