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New preparation method for 4-hydroxyl-beta-nitrostyrolene

A technology of nitrostyrene and p-hydroxybenzaldehyde, which is applied in the field of medicine and can solve the problems of low yield, unstable yield, complex synthesis process, etc.

Inactive Publication Date: 2018-10-09
SHANGHAI HUAJIN BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The yield of the existing 4-hydroxy-β-nitrostyrene preparation method is not high, the synthesis process is complicated, and the yield is unstable. It is necessary to invent a new preparation method to overcome the deficiencies of the existing technology, in order to achieve energy saving , environmental protection, green purpose

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0007] Embodiment 1: Preparation of 4-hydroxyl-beta-nitrostyrene:

[0008] Add 1221 mg of p-hydroxybenzaldehyde in the reactor, add 30 ml of methanol, stir, add 671 mg of nitromethane at room temperature, then stir in ice bath for 20 minutes, then add 848 mg of ammonium acetate, then stir at room temperature for 4 hours , the reaction solution gradually turned yellow. After standing for 5 hours, the yellow solid was filtered off. Then recrystallize in methanol, filter and dry in vacuum to obtain the compound 4-hydroxy-β-nitrostyrene with a yield of 91.1%.

Embodiment 2

[0009] Embodiment 2: Preparation of 4-hydroxyl-beta-nitrostyrene:

[0010] Add 1221 mg of p-hydroxybenzaldehyde in the reactor, add 30 ml of methanol, stir, add 671 mg of nitromethane at room temperature, then stir in ice bath for 20 minutes, then add 848 mg of ammonium acetate, then stir at room temperature for 4 hours , the reaction solution gradually turned yellow. After standing for 5 hours, the yellow solid was filtered off. Then recrystallize in methanol, filter and dry in vacuum to obtain the compound 4-hydroxy-β-nitrostyrene with a yield of 87.9%.

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PUM

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Abstract

The invention discloses a new preparation method for 4-hydroxyl-Beta-nitrostyrolene, and belongs to the technical field of medical technologies. The invention relates to a more advanced new preparation method for the 4-hydroxyl-Beta-nitrostyrolene. The key point of the technical scheme is a new preparation method for the compound. The formula is shown in the specification.

Description

technical field [0001] The invention relates to the technical field of medicine, in particular, the invention relates to a new preparation method of 4-hydroxy-β-nitrostyrene. Background technique [0002] 4-Hydroxy-β-nitrostyrene is an important intermediate raw material for the synthesis of pharmaceutical products. [0003] The yield of the existing 4-hydroxy-β-nitrostyrene preparation method is not high, the synthesis process is complicated, and the yield is unstable. It is necessary to invent a new preparation method to overcome the deficiencies of the existing technology, in order to achieve energy saving , environmental protection, green purposes. Contents of the invention [0004] The present invention adopts a new technology, aiming at the shortcomings of the existing 4-hydroxy-β-nitrostyrene preparation method that the yield is not high, the synthesis process is complicated, the yield is unstable, and the purchase cost of the required raw materials is high. Long-...

Claims

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Application Information

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IPC IPC(8): C07C201/06C07C205/17
CPCC07C201/06C07C205/17
Inventor 不公告发明人
Owner SHANGHAI HUAJIN BIOTECH CO LTD
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