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Preparation method of 2-amino-5-methylpyridine

A technology of picoline and amino, which is applied in the field of preparation of 2-amino-5-picoline, can solve the problems of high pressure in the treatment of three wastes, many reaction steps, and difficulty in realizing industrial production, and achieve less three wastes and fewer reaction steps Effect

Pending Publication Date: 2022-04-29
上海泾维化工科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the disadvantage is that there are many reaction steps, a large amount of waste water and waste gas are produced, and the pressure of the three wastes is high.
In addition, the third step reaction uses concentrated hydrobromic acid at a temperature of 210°C, which will cause serious corrosion to the equipment and make it difficult to realize industrial production

Method used

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  • Preparation method of 2-amino-5-methylpyridine
  • Preparation method of 2-amino-5-methylpyridine
  • Preparation method of 2-amino-5-methylpyridine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Add 800mL N, N-dimethylaniline, 93.6g (2.4mol) NaNH 2 , 7.0 g 2-amino-5-picoline. N 2 After replacing the air in the kettle twice, stir and heat up to 143°C, N 2 The pressure is 32kg / cm 2 .

[0048] 186.3g (2.0mol) of 3-methylpyridine was evenly pressed into the kettle for reaction within 5 hours with a pressurized metering pump, and the reaction temperature was controlled at 147-151°C. As the reaction progresses, the pressure in the kettle rises slowly, generally at 70kg / cm 2 the following. If the internal pressure exceeds 70kg / cm 2 , the vent valve can be slightly opened to keep the internal pressure at 70kg / cm 2 the following.

[0049] After adding 3-picoline, then at 147~151℃, pressure 66-70kg / cm 2Under reaction 5hr. Then cool down to below 35°C, vent the residual gas in the kettle, and use N 2 Substitution twice to remove the generated H 2 .

[0050] Remain 45g of reaction liquid in 2 liters of stainless steel pressure reactors, transfer the rest of th...

Embodiment 2

[0055] In 2 liters of stainless steel pressurized reactors, add the 45g reaction solution before hydrolysis reserved in the reserved examples, 800mLN, N-dimethylaniline, 93.6g (2.4mol) NaNH 2 . N 2 Warm up to 145°C after replacement, N 2 The pressure is 32kg / cm 2 . 186.3g (2.0mol) of 3-methylpyridine was evenly pressed into the kettle for reaction within 5 hours with a pressurized metering pump, and the reaction temperature was controlled at 147-151°C. As the reaction progresses, the pressure in the kettle rises slowly, generally at 70kg / cm 2 the following. If the internal pressure exceeds 70kg / cm 2 , the vent valve can be slightly opened to keep the internal pressure at 70kg / cm 2 the following.

[0056] After adding 3-picoline, then at 147~151℃, pressure 66-70kg / cm 2 Under reaction 5hr. Then cool down to below 35°C, vent the residual gas in the kettle, and use N 2 Substitution twice to remove the generated H 2 .

[0057] In 2 liters of stainless steel pressure re...

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Abstract

The invention relates to a preparation method of 2-amino-5-methylpyridine, which comprises the following steps: S1, sequentially adding reserved reaction liquid before hydrolysis, a solvent and sodium amide into a pressurized reaction kettle, replacing air in the kettle with N2, and heating to 140-160 DEG C; s2, under the pressure of 30-40kg / cm < 2 >, adding 3-methylpyridine into the reaction kettle for reaction, and then reacting for 2-6 hours; s3, after the reaction is finished, cooling to below 35 DEG C, emptying residual gas in the kettle, then replacing the residual gas in the kettle with N2, adding water to carry out hydrolysis reaction, and then reacting for 1 hour; and S4, carrying out phase splitting on the material after complete reaction in the step S3, extracting the obtained water phase, combining with the organic phase, and then distilling to obtain the product. The invention relates to an improved Chieliabin reaction method, the total yield of the prepared product can reach 87.7%, and the yield of 2-amino-5-methylpyridine can reach 71.2%.

Description

technical field [0001] The invention belongs to the technical field of preparation of fine chemical intermediates, and in particular relates to a preparation method of 2-amino-5-picoline. Background technique [0002] 2-Amino-5-picoline is an intermediate in the synthesis of high-efficiency, low-toxicity and broad-spectrum insecticides imidacloprim and ethetamiprid, and is widely used in the synthesis of nicotinic compounds. Some functional dyes are also synthesized with subs. [0003] According to literature reports, 2-amino-5-picoline has the following preparation methods. [0004] In 1983, the patent published by Reilly Industries of the United States disclosed that 2-amino-5-picoline was prepared by Chichibabin reaction using 3-picoline and sodium amide as raw materials, and at the same time, the pharmaceutical intermediate 2-amino-3 -The method of picoline (hereinafter referred to as 2,3-isomer). The reaction formula is as follows: [0005] [0006] The advantage...

Claims

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Application Information

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IPC IPC(8): C07D213/73
CPCC07D213/73
Inventor 姚虎生王良锋吴亦初赵珠琳
Owner 上海泾维化工科技有限公司
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