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Synthetic method of N-methylpiperidine

A technology of methyl piperidine and a synthesis method, which is applied in the synthesis field of N-methyl piperidine, can solve the problems of serious pollution, complicated operation, large energy consumption and the like, and achieves a reaction with less impurities, simple operation and low energy consumption. Effect

Inactive Publication Date: 2017-12-01
李怡舒 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The present invention aims at problems such as large energy consumption existing in the production of N-methylpiperidine, low yield, serious pollution, complicated operation, etc., and provides a kind of synthetic method of N-methylpiperidine, reacts and obtains N through filtration and distillation -Methylpiperidine, with high purity, can be used directly without purification, and the remaining solid is potassium dihydrogen phosphate, which can be recycled and directly used as fertilizer

Method used

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Examples

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Effect test

Embodiment 1

[0026] Weigh 170g of piperidine in a 500mL three-neck flask with mechanical stirring, heat it to 80°C in an oil bath, weigh 72g of paraformaldehyde and 144g of potassium dihydrogen phosphite, mix well, and then add them to piperidine in batches , the total addition time is controlled within 1h, divided into 4 batches, and the interval between each batch is 15 minutes. During the addition process, attention should be paid to prevent flushing; after the addition is completed, react for 2 hours. After the piperidine reaction is complete by thin-layer chromatography, cool to room temperature. 130g of filtrate and residue were obtained by suction filtration, and the residue obtained by suction filtration was placed in a reaction flask and heated to 110°C for distillation until no liquid was distilled out. The remaining solid after distillation was potassium dihydrogen phosphate 128g, which was recovered and used as fertilizer, Liquid is 54g, and the composition of filtrate and disti...

Embodiment 2

[0028] Weigh 170g of piperidine in a 500mL three-necked flask with mechanical stirring, heat it to 90°C in an oil bath, weigh 72g of paraformaldehyde and 144g of potassium dihydrogen phosphite, mix well, and then add them to piperidine in batches , the total addition time is controlled within 1.5h, divided into 6 batches in total, and the interval between each batch is 15 minutes. During the addition, attention should be paid to prevent flushing; after the addition is completed, the reaction is 1.5h. After the piperidine reaction is complete by thin-layer chromatography, it is cooled to At room temperature, 140g of filtrate and residue were obtained by suction filtration; the residue obtained by suction filtration was placed in a reaction flask and heated to 115°C for distillation until no liquid was distilled out. The remaining solid after distillation was potassium dihydrogen phosphate 126g, which was recovered and used as a fertilizer. Distillate is 46g, and the composition ...

Embodiment 3

[0030] Weigh 170g of piperidine in a 500mL three-neck flask with mechanical stirring, heat it in an oil bath to 100°C, weigh 72g of paraformaldehyde and 144g of potassium dihydrogen phosphite, mix well, and then add them to piperidine in batches , the total addition time is controlled within 50 minutes, divided into 5 batches, and the interval between each batch of addition is 10 minutes. During the addition process, attention should be paid to prevent flushing; after the addition is completed, the reaction is 2.5h. After the piperidine reaction is complete by thin-layer chromatography, it is cooled to At 60°C, 152g of filtrate and residue were obtained by suction filtration; the residue obtained by suction filtration was placed in a reaction flask and heated to 120°C for distillation until no liquid was distilled out. The remaining solid after distillation was potassium dihydrogen phosphate 122g, which was recovered and used as fertilizer , distillate is 36g, and the compositi...

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Abstract

The invention provides a synthetic method of N-methylpiperidine. The synthetic method comprises the steps of heating piperidine to 80-100 DEG C, adding paraformaldehyde and potassium dihydrogen phosphite to react, filtering to obtain N-methylpiperidine and a solid, heating and distilling the obtained solid, and collecting distillate, namely N-methylpiperidine, wherein the molar ratio of piperidine to paraformaldehyde to potassium dihydrogen phosphate is 1 to (1-1.2) to (0.5-0.6). N-methylpiperidine prepared through filtration and distillation is high in purity and can be directly utilized without being purified, and the residual solid is potassium dihydrogen phosphate and can be directly recycled to be used as a fertilizer.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a synthesis method of N-methylpiperidine. Background technique [0002] The plant growth regulator methylpiperium can promote the reproductive growth of plants, inhibit the crazy growth of stems and leaves, control side branches, increase the number and vitality of roots, and increase the stress resistance of plants, especially when used on cotton, it can effectively prevent the crazy growth of cotton, control plant It is compact in shape, reduces boll drop, promotes maturation, increases cotton yield, and has little toxic residue of mepiperium. my country is a large agricultural country, and N-methylpiperidine is an important intermediate in the synthesis of mepiperium, and its synthesis has a huge role in promoting the development of agriculture. [0003] The synthetic method of N-methylpiperidine mainly contains following two kinds at present: [0004] ...

Claims

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Application Information

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IPC IPC(8): C07D295/03C07D295/023
CPCC07D295/023C07D295/03
Inventor 李怡舒郑义丁群山郑先福
Owner 李怡舒
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