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High-efficiency green synthesis method for p-methoxypropiophenone

A methoxyphenyl ethyl ketone, green synthesis technology, applied in chemical instruments and methods, condensation preparation of carbonyl compounds, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of expensive catalysts and high yields. It can not meet the market demand and other problems, and achieve the effect of low cost, high product yield and high catalyst activity

Inactive Publication Date: 2018-04-20
SUZHOU GAIDE FINE MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the yield of this method also can't reach market demand, and catalyst price is more expensive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The efficient green synthetic method of p-methoxyphenyl ethyl ketone comprises the following steps:

[0026] (1) Using deionized water as a solvent, prepare iron salt solution, manganese salt solution, zirconium salt solution;

[0027] (2) prepare the mixed solution of sodium citrate, sodium salicylate;

[0028] (3) Mix the iron salt solution, manganese salt solution, and zirconium salt solution prepared above with the mixed solution of sodium citrate and sodium salicylate, stir and mix at 3000rpm for 10min, and prepare mixed solution A; wherein, The mass ratio of the mixed solution of iron salt solution, manganese salt solution, zirconium salt solution and sodium citrate, sodium salicylate is 11:7:10:5;

[0029] (4) Prepare an aqueous solution of sodium hydroxide; and add it dropwise to the mixed solution A prepared above, and stir while adding dropwise. After the dropwise addition, slowly raise the temperature to 40° C., and treat it with constant temperature stirrin...

Embodiment 2

[0033] The efficient green synthetic method of p-methoxyphenyl ethyl ketone comprises the following steps:

[0034] (1) Using deionized water as a solvent, prepare iron salt solution, manganese salt solution, zirconium salt solution;

[0035] (2) prepare the mixed solution of sodium citrate, sodium salicylate;

[0036] (3) Mix the iron salt solution, manganese salt solution, and zirconium salt solution prepared above with the mixed solution of sodium citrate and sodium salicylate, stir and mix at 3000rpm for 10min, and prepare mixed solution A; wherein, The mass ratio of the mixed solution of iron salt solution, manganese salt solution, zirconium salt solution and sodium citrate, sodium salicylate is 11:7:10:5;

[0037] (4) Prepare an aqueous solution of sodium hydroxide; and add it dropwise to the mixed solution A prepared above, and stir while adding dropwise. After the dropwise addition, slowly raise the temperature to 40° C., and treat it with constant temperature stirrin...

Embodiment 3

[0041] The efficient green synthetic method of p-methoxyphenyl ethyl ketone comprises the following steps:

[0042] (1) Using deionized water as a solvent, prepare iron salt solution, manganese salt solution, zirconium salt solution;

[0043] (2) prepare the mixed solution of sodium citrate, sodium salicylate;

[0044] (3) Mix the iron salt solution, manganese salt solution, and zirconium salt solution prepared above with the mixed solution of sodium citrate and sodium salicylate, stir and mix at 3000rpm for 10min, and prepare mixed solution A; wherein, The mass ratio of the mixed solution of iron salt solution, manganese salt solution, zirconium salt solution and sodium citrate, sodium salicylate is 11:7:10:5;

[0045](4) Prepare an aqueous solution of sodium hydroxide; and add it dropwise to the mixed solution A prepared above, and stir while adding dropwise. After the dropwise addition, slowly raise the temperature to 40° C., and treat it with constant temperature stirring...

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Abstract

The invention discloses a high-efficiency green synthesis method for p-methoxypropiophenone. The synthesis method specifically comprises the following steps: firstly, preparing a composite catalyst byusing an iron salt solution, a manganese salt solution and a zirconium salt solution as raw materials; mixing p-methoxybenzoic acid and propionic acid, carrying out uniform stirring, then transferring the obtained mixture to a four-necked flask, adding the prepared composite catalyst, carrying out stirring for 5min, slowly raising the temperature to 130+ / -5 DEG C, carrying out a constant-temperature stirring reflux reaction for 5h, distilling off excess propionic acid, continuing to carry out heating to 270 DEG C, carrying out a constant-temperature stirring reaction, absorbing escaped gas and distilled liquid by using an ethanol solution, wherein when no liquid is distilled out, the reaction is finished, then carrying out cooling and crystallizing to obtain the p-methoxypropiophenone. The catalyst adopted by the method of the invention has large catalytic activity, the reaction time is effectively shortened, the yield of the target product is high, and the preparation cost is low.

Description

Technical field: [0001] The invention relates to the field of preparation of pharmaceutical intermediates, in particular to an efficient green synthesis method of p-methoxyphenyl ethyl ketone. Background technique: [0002] P-methoxyphenyl ethyl ketone is an important pharmaceutical intermediate, used in the production of respiratory system drugs formoterol and β-phenylethylamine, heart and brain system drugs amphetamine and lactic acid cardiodine and hormone drugs phenyl Isopropylamine etc. At present, this product has not been produced on a large scale in China, and its purity is only 95%, which cannot meet the market demand. [0003] Patent 201110155185.X discloses a preparation method of p-methoxypropiophenone, a pharmaceutical intermediate, which specifically includes the following steps: using p-methoxybenzoic acid and propionic acid as raw materials, reacting in the presence of a composite catalyst to prepare p-methoxypropiophenone Methoxypropiophenone; the composit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/48C07C49/84B01J23/889
CPCC07C45/48B01J23/002B01J23/8892B01J37/03B01J37/10B01J2523/00B01J2523/48B01J2523/72B01J2523/842C07C49/84
Inventor 李晓明
Owner SUZHOU GAIDE FINE MATERIALS CO LTD
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