Method for continuous preparation of 2-chloro-5-chloromethylpyridine in microchannel

The technology of chloromethylpyridine and picoline, which is applied in the field of preparation of 2-chloro-5-chloromethylpyridine, can solve the problems of high raw material price, long reaction steps, unsatisfactory cyclization reaction yield and the like, To achieve the effect of simple preparation, short production cycle, continuous stability

Active Publication Date: 2012-11-28
广西绿友农生物科技股份有限公司
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Problems solved by technology

However, the synthesis method has long reaction steps, hig

Method used

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  • Method for continuous preparation of 2-chloro-5-chloromethylpyridine in microchannel
  • Method for continuous preparation of 2-chloro-5-chloromethylpyridine in microchannel
  • Method for continuous preparation of 2-chloro-5-chloromethylpyridine in microchannel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1 (optimal process conditions)

[0026] Mix 6.38g (0.05mol) 2-chloro-5-methylpyridine and 0.1g (0.0006mol) azobisisobutyronitrile (AIBN) in 12.5ml chlorobenzene to prepare 2-chloro-5-methyl The final concentration of pyridine is 0.003mol / ml mixed solution, as sample solution A; measure sulfuryl chloride SO 2 Cl 2 3.38g (0.025mol), dissolved in 16ml of chlorobenzene to form a mixed solution of sulfonyl chloride with a final concentration of 0.0015mol / ml, as sample B. The calibrated syringe pumps (model LSP01-1A, manufacturer: Baoding Lange Constant Flow Pump Co., Ltd.) of sample solution A and sample solution B are sent to the microchannel reactor with a total flow rate of 2.0m / min. Before raising the temperature of the microchannel reactor to 110℃, the residence time of sample A and sample B in the microchannel reactor (a polytetrafluoroethylene tube with inner diameter D=0.6mm and length L=2m) is 60s, and collect The effluent from the outlet of the microchannel r...

Embodiment 2

[0030] Sample solution A and sample solution B are the same as in Example 1; sample solution A and sample solution B are injected into the microchannel reactor at a certain flow rate for reaction. The total flow rate, reaction temperature, residence time, inner diameter and other process parameters are shown in Table 2. Collect the effluent reaction solution to obtain the reaction solution of 2-chloro-5-chloromethylpyridine. The single-pass yield is over 30~68% by gas chromatography (model: GC-14B, manufacturer: Japan Shimadzu). The selectivity of the product 2-chloro-5-chloromethylpyridine is 90~99%, as shown in Table 2.

[0031] Table 2 The influence of the better process conditions on the reaction

[0032]

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Abstract

The invention discloses a method for continuous preparation of 2-chloro-5-chloromethylpyridine in a microchannel. The method consists of: taking 2-chloro-5-methylpyridine as a raw material, adopting sulfonyl chloride as a chlorinating reagent, employing azodiisobutyronitrile as an initiator, and using an organic solvent as a reaction medium, in a microchannel reactor, conducting a chlorination reaction under 80-130DEG C, controlling the retention time of the reaction by controlling the flow rate of a reaction solution, and after the reaction, collecting the effluent of the microchannel reactor, thus obtaining the 2-chloro-5-chloromethylpyridine. The method disclosed in the invention greatly shortens the reaction time, improves the reaction efficiency and the product quality, and makes the product selectivity up to 97.88%. The reaction system in the invention has no amplification effect, can realize amplification by several times through parallel connection, and has the advantages of continuous reaction stability, simple operation, short production cycle, cheap and easily available raw materials, simple production process and the like, thus being suitable for industrialized production.

Description

(1) Technical field [0001] The invention relates to a method for preparing 2-chloro-5-chloromethylpyridine, in particular to a method for continuously preparing 2-chloro-5-chloromethylpyridine in a microchannel reactor. (2) Background technology [0002] 2-chloro-5-chloromethylpyridine (2-chloro-5-chloromethylpyridine, referred to as CCMP) is the key intermediate of the new high-efficiency pesticides Imidacloprid (Imidacloprid) and Imidacloprid (NI-25), as well as this type of pesticide molecule The most insecticidal active part of it. And through its alkylation reaction, condensation reaction with heterocyclic N-H, and reaction with 1-nitro-2,2-bis(thiomethyl)ethylene after amination, a series of new insecticides can be prepared Acaricide. [0003] There are more than 10 synthetic processes developed so far, but few can be used in industrial production. The synthetic routes can be divided into two categories: directly from pyridine and its derivatives through chlorination or di...

Claims

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Application Information

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IPC IPC(8): C07D213/61
Inventor 余武斌高建荣郑明明陈晓萍叶青
Owner 广西绿友农生物科技股份有限公司
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