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New preparation method of 3,4-dyhydroxyl-Beta-nitrostyrolene

A technology of nitrostyrene and dihydroxybenzaldehyde, applied in the field of medicine, can solve the problems of low yield, unstable yield, complex synthesis process and the like

Inactive Publication Date: 2018-11-13
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 3,4-dihydroxy-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 prior art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0007] Embodiment 1: Preparation of 3,4-dihydroxy-β-nitrostyrene:

[0008] Add 1381 mg of 3,4-dihydroxybenzaldehyde in the reactor, add 35 ml of methanol, stir, add 671 mg of nitromethane at room temperature, then stir in an ice bath for 20 minutes, then add 848 mg of ammonium acetate, and then After stirring at room temperature for 4 hours, the reaction solution gradually turned yellow. After standing for 5 hours, the yellow solid was filtered off. Then recrystallized in methanol, filtered and dried in vacuum to obtain compound 3,4-dihydroxy-β-nitrostyrene with a yield of 83.7%.

Embodiment 2

[0009] Embodiment 2: Preparation of 3,4-dihydroxy-β-nitrostyrene:

[0010] Add 1381 mg of 3,4-dihydroxybenzaldehyde in the reactor, add 35 ml of methanol, stir, add 671 mg of nitromethane at room temperature, then stir in an ice bath for 20 minutes, then add 848 mg of ammonium acetate, and then After stirring at room temperature for 4 hours, the reaction solution gradually turned yellow. After standing for 5 hours, the yellow solid was filtered off. Then recrystallized in methanol, filtered and dried in vacuum to obtain compound 3,4-dihydroxy-β-nitrostyrene with a yield of 87.1%.

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PUM

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Abstract

The invention discloses a new preparation method of 3,4-dyhydroxyl-Beta-nitrostyrolene, and belongs to the technical field of medicine technologies. A technical problem to be solved relates to a moreadvanced new preparation method of the 3,4-dyhydroxyl-Beta-nitrostyrolene. The key point of the technical problem to be solved is a new preparation method of a compound.

Description

technical field [0001] The invention relates to the technical field of medicine, in particular, the invention relates to a new preparation method of 3,4-dihydroxy-β-nitrostyrene. Background technique [0002] 3,4-Dihydroxy-β-nitrostyrene is an important intermediate raw material for the synthesis of pharmaceutical products. [0003] The yield of the existing 3,4-dihydroxy-β-nitrostyrene is not high, the synthesis process is complex, and the yield is unstable. It is necessary to invent a new preparation method to overcome the shortcomings of the existing technology. Contents of the invention [0004] The present invention adopts a new technology, aiming at the low yield of the existing 3,4-dihydroxy-β-nitrostyrene preparation method, complex synthesis process, unstable yield and high purchase cost of required raw materials Disadvantages: After long-term research and development, a new preparation method was invented to overcome the deficiencies of existing technologies and...

Claims

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Application Information

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IPC IPC(8): C07C201/12C07C205/17
CPCC07C201/12C07C205/17
Inventor 不公告发明人
Owner SHANGHAI HUAJIN BIOTECH CO LTD
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