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Preparation method of N, N-dimethyl piperidine chloride salt

A technology of dimethylpiperidine and chloride salt, which is applied in the field of preparation of N,N-dimethylpiperidine chloride salt, can solve the problems of poor operation safety, low product content, and low yield, and achieve low cost, High yield and content, safe operation

Active Publication Date: 2019-05-24
鹤壁全丰生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, the synthesis of N,N-dimethylpiperidinium chloride salt has problems such as low product content, poor operation safety, and low yield.

Method used

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  • Preparation method of N, N-dimethyl piperidine chloride salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1, the preparation of N,N-dimethyl piperidine chloride salt

[0025] Take 80g of 25% NaOH solution, 160g of n-butanol, and 40g of piperidine into a 500mL autoclave in sequence. After sealing it, put 55g of methyl chloride into it, react at 70°C for 4h, release the material and transfer it to a 500mL distillation bottle, and adjust the vacuum to - 0.07MPa, heat up to 70°C to evaporate 43g of water, then adjust the temperature to 60°C for filtration, filter out sodium chloride, transfer the filtrate to a 500mL pear-shaped flask, and use rotary thin-film evaporation at -0.09MPa, 85°C The device evaporates the material to dryness. The temperature was lowered to 25° C. to obtain 69 g of product with a content of 99.6% and a yield of 98.7%.

Embodiment 2

[0026] Embodiment 2, the preparation of N,N-dimethyl piperidine chloride salt

[0027] Take 95g of 20% NaOH solution, 120g of isobutanol, and 40g of piperidine into a 500mL autoclave in sequence, and then put 55g of methyl chloride into the autoclave after sealing, react at 65°C for 5h, release the material and transfer it to a 500mL distillation bottle, and adjust the vacuum to - 0.06MPa, heat up to 70°C to evaporate 64g of water, then adjust the temperature to 50°C for filtration, filter out sodium chloride, transfer the filtrate to a 500mL pear-shaped flask, and use rotary thin-film evaporation at -0.09MPa, 75°C The device evaporates the material to dryness. The temperature was lowered to 25° C. to obtain 69.5 g of product with a content of 99.3% and a yield of 99.1%.

Embodiment 3

[0028] Embodiment 3, the preparation of N,N-dimethyl piperidine chloride salt

[0029] Take 65g of 30% NaOH solution, 200g of n-butanol, and 40g of piperidine into a 500mL autoclave in sequence, and after sealing it, put 55g of methyl chloride into it, react at 60°C for 5h, release the material and transfer it to a 500mL distillation bottle, and adjust the vacuum to - 0.07MPa, heat up to 70°C to evaporate 30g of water, then adjust the temperature to 60°C for filtration, filter out sodium chloride, transfer the filtrate to a 500mL pear-shaped bottle, and use rotary thin-film evaporation at -0.09MPa, 85°C The device evaporates the material to dryness. The temperature was lowered to 25° C. to obtain 69.2 g of product with a content of 99.1% and a yield of 98.5%.

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Abstract

The invention discloses a preparation method of N, N-dimethyl piperidine chloride salt. The method comprises the following steps: adding alkali liquor, a solvent and piperidine into a closed reactioncontainer, then introducing methyl chloride, and heating for reaction to obtain the N, N-dimethyl piperidine chloride salt. According to the method, the high-purity N, N-dimethyl piperidine chloride salt (with the content greater than 99%) can be synthesized; side reaction hardly occurs in the reaction process, SN2 main reaction is very thorough, and water can be separated from a reaction system;and the solubility of the N, N-dimethyl piperidinium chloride salt in the system is small at low temperature, and thus, the N, N-dimethyl piperidinium chloride salt is separated from the system favorably. The yield and content of the N, N-dimethyl piperidinium chloride salt are quite high; and the preparation method is safe to operate and low in cost.

Description

technical field [0001] The invention relates to a preparation method of N,N-dimethylpiperidine chloride salt, which belongs to the field of fine chemical synthesis. Background technique [0002] N, N dimethyl piperidine chloride is a plant growth regulator with high efficiency, low toxicity and no phytotoxicity. It can promote the reproductive growth of plants, control side branches, inhibit the crazy growth of stems and leaves, increase the number and vitality of roots, and increase the weight of fruits. The product is widely used in cotton, wheat, rice, peanut, potato, grape, vegetable, beans and other crops. [0003] The industrial production method of N,N dimethylpiperidine chloride salt used to prepare N-methylpiperidine by reacting formaldehyde, formic acid and piperidine, and then add it to monochloromethane to produce N-methylpiperidine. Great that craft has been eliminated. [0004] At present, the synthesis process of N,N dimethylpiperidine chloride salt in indu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/06
Inventor 陈云生张朋飞谢三星
Owner 鹤壁全丰生物科技有限公司
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