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A kind of 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 low yield, low product content, poor operation safety, etc., and achieve yield and The effect of high content, safe operation and low cost

Active Publication Date: 2020-10-16
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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  • A kind of preparation method of n,n-dimethyl piperidine chloride salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1. Preparation of N,N-dimethylpiperidine chloride salt

[0025] Take 80g of 25% NaOH solution, 160g of n-butanol, and 40g of piperidine into the 500mL autoclave in turn, and then pass in 55g of methyl chloride and react at 70℃ for 4h. The material is released and transferred to a 500mL distillation flask, and the vacuum is adjusted to- 0.07MPa, heat up to 70°C and steam 43g of water, then adjust the temperature to 60°C for filtration, filter out the sodium chloride, transfer the filtrate to a 500mL pear-shaped bottle, and evaporate with a rotary film at -0.09MPa and 85°C The material is evaporated 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] Example 2. Preparation of N,N-dimethylpiperidine chloride salt

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

Embodiment 3

[0028] Example 3. Preparation of N,N-dimethylpiperidine chloride salt

[0029] Take 65g of 30% NaOH solution, 200g of n-butanol, and 40g of piperidine into 500mL autoclave successively. After airtight, 55g of methyl chloride is introduced, reacted at 60℃ for 5h, the material is released and transferred to a 500mL distillation flask, and the vacuum is adjusted to- 0.07MPa, heat up to 70°C and steam 30g of water, then adjust the temperature to 60°C for filtration, filter out the sodium chloride, transfer the filtrate to a 500mL pear-shaped bottle, and evaporate on a rotary film at -0.09MPa and 85°C The material is evaporated to dryness. The temperature was lowered to 25°C to obtain 69.2 g of product, the content was 99.1%, and the yield was 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 salt is a highly effective, low-toxic, non-phytotoxic plant growth regulator. It can promote the reproductive growth of plants, control side branches, inhibit the crazy growth of stems and leaves, improve root coefficient and vitality, and increase fruit weight. This product is widely used in crops such as cotton, wheat, rice, peanuts, potatoes, grapes, vegetables, beans and so on. [0003] The industrial production method of N,N dimethyl piperidine chloride salt used to produce N-methyl piperidine by reacting formaldehyde, formic acid and piperidine, and then adding it with monochloromethane. The process has been eliminated. [0004] At present, the industrial synthesis process of N,N dimethyl piperidine chloride salt is mainly a three-step method: firstly...

Claims

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Application Information

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Patent Type & Authority Patents(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