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Method for preparing 2,3,5-trimethylpyridine

A collidine and lutidine technology, applied in 2 fields, can solve the problems of low synthesis yield, harsh reaction conditions, and high cost, and achieve the effects of simple preparation process, low raw material cost, and high production efficiency

Inactive Publication Date: 2007-08-08
ZHEJIANG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Wherein, the first method has many by-products, the yield of 2,3,5-collidine is very low, and the separation is more difficult, which makes the cost higher; the basic raw material used in the second ring closure of the method is ethyl 2-methylacetoacetate and 2-methyldiethylmalonate, the raw materials are not easy to obtain, while the process route is longer, and the noble metal palladium is used as a catalyst, the total yield is 59.4%, and the cost is high; the shortcoming of method three is that methyllithium is very expensive , and it will decompose when encountering water or oxygen, the reaction conditions are harsh, and 3,5-lutidine is difficult to obtain, so it cannot be used in industrial production; the raw material 2-ethyl-3,5-dimethylpyridine used in method four Pyridine, the price is more expensive, the synthesis yield is relatively low, the highest is 30%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The first step prepares the cobalt-aluminum phosphate catalyst that contains acid regulator

[0015] Dissolve 81.2g (NH 4 ) 3 PO 4 ·3H 2 O crystal, weigh 20.3g of basic alumina and pour it into a 1000mL flask, add about 250mL of deionized water and stir, dissolve 54.9g of cobalt nitrate and 42.6g of aluminum nitrate in 250mL of distilled water, slowly drop them into the prepared Contains (NH 4 ) 3 PO 4 Put the solution in a flask, stir for 30 minutes, filter the formed precipitate with suction, wash the filter cake with 4×200mL de-distilled water, dry the filter cake properly, and then bake it at 400°C for 12 hours before use.

[0016] In the second step, propionaldehyde and ammonia are used as raw materials for ring-forming reaction

[0017] Add a certain amount of catalyst into the fixed-bed reactor, raise the temperature to 450°C, control the injection speed of ammonia gas at about 200mL / min, turn on the injection pump, and adjust the injection speed of propio...

Embodiment 2

[0023] The first step prepares the cobalt-aluminum phosphate catalyst that contains acid regulator

[0024] Dissolve 81.2g (NH 4 ) 3 PO 4 ·3H 2 O crystal, weigh 32.5g of basic alumina and pour it into a 1000mL flask, add about 250mL of deionized water and stir, dissolve 54.9g of cobalt nitrate and 42.6g of aluminum nitrate in 250mL of distilled water, slowly drop them into the prepared Contains (NH 4 ) 3 PO 4 Put the solution in a flask, stir for 30 minutes, filter the formed precipitate with suction, wash the filter cake with 4×200mL de-distilled water, dry the filter cake properly, and then bake it at 400°C for 12 hours before use.

[0025] In the second step, propionaldehyde and ammonia are used as raw materials for ring-forming reaction

[0026] Add a certain amount of catalyst into the fixed-bed reactor, raise the temperature to 380°C, control the injection speed of ammonia gas at about 200mL / min, turn on the injection pump, and adjust the injection speed of propio...

Embodiment 3

[0032] The first step prepares the cobalt-aluminum phosphate catalyst that contains acid regulator

[0033] Dissolve 81.2g (NH4 ) 3 PO 4 ·3H 2 O crystal, weigh 40.6g of basic silica and pour it into a 1000mL flask, add about 250mL of deionized water and stir, dissolve 54.9g of cobalt nitrate and 42.6g of aluminum nitrate in 250mL of distilled water, slowly drop them into the prepared Contains (NH 4 ) 3 PO 4 Put the solution in a flask, stir for 30 minutes, filter the formed precipitate with suction, wash the filter cake with 4×200mL de-distilled water, dry the filter cake properly, and then bake it at 400°C for 12 hours before use.

[0034] In the second step, propionaldehyde and ammonia are used as raw materials for ring-forming reaction

[0035] Add a certain amount of catalyst into the fixed-bed reactor, raise the temperature to 300°C, control the injection speed of ammonia gas at about 200mL / min, turn on the injection pump, and adjust the injection speed of propional...

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PUM

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Abstract

The invention discloses a making method of 2, 3, 5-trimethyl pyridine, which comprises the following steps: 1) making composite catalyst of cobalt aluminium phosphate with acid degree adjuster; 2) placing the composite catalyst into fixed bed reactor; aerating propanal and ammonia gas; looping to generate 2-ethyl-3, 5-dimethyl pyridine; 3) demethylating 2-ethyl-3, 5-dimethyl pyridine and sulfur flour; obtaining the product.

Description

technical field [0001] The invention relates to a preparation method of 2,3,5-collidine. Background technique [0002] 2,3,5-collidine is an intermediate for preparing H+ / K+-ATPase inhibitors omeprazole and tetuprazole for treating peptic ulcer. Existing 2,3,5-collidine main preparation method has following several kinds: method one (Uzb.Khim.Zh.1990, (1), 29~31), with propionaldehyde and ammonia in Zn-Cr -In the presence of an Al catalyst, react at 380°C under normal pressure conditions, the resulting product contains 27.6% of 2,3,5-collidine and 31.1% of 2-ethyl-3,5-lutidine; method Two (Japanese Open Patent 87-72666), this method is to obtain 3-amino-2-methyl-2-butenoic acid ethyl ester by 2-methyl acetoacetate and liquefied ammonia reaction in autoclave, then 2 -Diethyl methylmalonate reacts with 3-amino-2-methyl-2-butenoic acid ethyl ester in the presence of sodium ethoxide to obtain 4-hydroxyl-3,5,6-trimethyl-2( 1H)-pyridone, and then react with phosphorus oxychlori...

Claims

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Application Information

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IPC IPC(8): C07D213/06
Inventor 陈英奇戴立言王晓钟李永进
Owner ZHEJIANG UNIV
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