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Separating method of 2-chloropyridine and 3-chloropyridine

A separation method, the technology of chloropyridine, applied in chemical instruments and methods, organic chemical methods, preparation of organic compounds, etc., can solve the problems of complex equipment, high operation risk factor, high energy consumption, etc., and achieve simple operation and safe operation Good, energy-saving effect

Active Publication Date: 2019-10-25
ZHEJIANG UNIV
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  • Application Information

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Problems solved by technology

[0008] Aiming at the problems of high energy consumption, complex equipment, high operating risk factor and the deficiencies in this field in the process of purifying 2-chloropyridine in industry, the present invention provides a method for separating 2-chloropyridine and 3-chloropyridine. Non-porous self-adaptive bis-dibromoethoxy column[6]arene crystal material for purification of 2-chloropyridine

Method used

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  • Separating method of 2-chloropyridine and 3-chloropyridine
  • Separating method of 2-chloropyridine and 3-chloropyridine
  • Separating method of 2-chloropyridine and 3-chloropyridine

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Embodiment 1

[0029] Preparation of bis-dibromoethoxypillar[6]arene crystal material: Bis-dibromoethoxypillar[6]arene was prepared using 1,1-dibromo-p-phenylenediethyl ether.

[0030] 1,1-Dibromo-p-phenylenediethyl ether (6.74 g, 23.0 mmol) was added to 100 mL of 1,2-dichloroethane, and BF 3 ·O(C 2 h 5 ) 2 (23.0~23.5mmol), the mixture was stirred at 25°C for 20~30 minutes, quenched with saturated sodium bicarbonate solution to end the reaction, washed twice with deionized water, and the organic phase was concentrated under reduced pressure to obtain the crude product, which was used for Purification by flash column chromatography (petroleum ether / dichloromethane volume ratio = 1:2) gave bis-dibromoethoxycolum[6]arene (1.20 g, 16.9% yield) as a white solid. The white solid was placed in a vacuum oven at 120° C. overnight to obtain the activated bis-dibromoethoxypillar[6]arene crystal material as a white powder, denoted as BrP6.

[0031] The product characterization data prepared in this ...

Embodiment 2

[0035] Adsorption of 2-chloropyridine or 3-chloropyridine by bis-dibromoethoxy column[6]arene crystal material: take two 20mL strain bottles, add 2mL 2-chloropyridine and 2mL 3-chloropyridine respectively, and name For BrP6@2-CP and BrP6@3-CP, respectively take 30mg of bis-dibromoethoxy column[6]arene crystal material and place them in two 5mL strain bottles, and place two open 5mL strain bottles in In two 20mL strain bottles, seal the 20mL strain bottles well, place them at room temperature at 25°C for 48 hours, and place the obtained powder in an oven at 40°C for 30 minutes.

[0036] The product characterization data prepared in this embodiment are as follows:

[0037] BrP6@2-CP, 1H NMR (400MHz, CDCl3, 298K, ppm) δ8.42–8.39 (m, 2H), 7.66 (td, J = 7.7, 2.0Hz, 2H), 7.34 (dt, J = 8.1, 0.9Hz, 2H), 7.23(ddd,J=7.4,4.9,1.0Hz,2H),6.78(s,12H),4.16(t,J=5.8Hz,24H),3.87(s,12H),3.55(t,J=5.8Hz ,24H).

[0038] BrP6@3-CP, 1 H NMR (400MHz, CDCl 3 ,298K,ppm)δ8.59(d,J=2.5Hz,2H),8.50(d,J=...

Embodiment 3

[0042] Adsorption of the mixture of 2-chloropyridine and 3-chloropyridine with a volume ratio of 1:1 by bis-dibromoethoxy column[6]arene crystal material: take a 20mL seed bottle, add 1mL 2-chloropyridine and 1mL 3 -Chloropyridine, named BrP6@2 / 3-CP, take 30mg of bisdiethoxy column[6]arene crystal material and place it in a 5mL strain bottle, and put the open 5mL strain bottle into the above 20mL strain bottle In the 20mL strain bottle, seal it well, and place it at room temperature at 25°C for 48 hours, and place the obtained powder in an oven at 40°C for 30 minutes.

[0043] The product characterization data prepared in this embodiment are as follows:

[0044] BrP6@2 / 3-CP, 1 H NMR (400MHz, CDCl 3 ,298K,ppm)δ8.40(dd,J=4.9,1.5Hz,2H),7.66(td,J=7.9,2.0Hz,2H),7.34(d,J=8.0Hz,2H),7.23(ddd ,J=7.4,4.9,0.9Hz,2H),6.78(s,12H),4.16(t,J=5.8Hz,24H),3.87(s,12H),3.55(t,J=5.8Hz,24H) .

[0045] exist 1 Only the signal of the hydrogen atom corresponding to 2-chloropyridine was found in th...

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Abstract

The invention discloses a separating method of 2-chloropyridine and 3-chloropyridine. A bis(dibromoethyoxypillar[6]arene) crystal material is used for adsorbing and separating a mixture of the 2-chloropyridine and the 3-chloropyridine, wherein a structural formula of the bis(dibromoethyoxypillar[6]arene) crystal material is as shown in the description. According to the separating method of the 2-chloropyridine and the 3-chloropyridine, the separating process is simple to operate, no complex equipment is needed, and the operation safety is good; no rectification operation is needed during separation, so that energy is saved, and the production cost is reduced; and the used crystal material is high in stability, and can be recycled, and a separating effect is not reduced.

Description

technical field [0001] The invention relates to the technical field of adsorption separation, in particular to a method for separating 2-chloropyridine and 3-chloropyridine. Background technique [0002] As a very important intermediate in industrial production, 2-chloropyridine is widely used in the fields of medicine, pesticide synthesis and daily chemical industry, and has broad market prospects. In recent years, with the continuous expansion of the application field of 2-chloropyridine market, the demand is also increasing, so it has been widely valued. [0003] At present, there are mainly three methods for industrially synthesizing 2-chloropyridine: N-oxidation method, photochlorination method, and thermal chlorination method. Among them, the thermal chlorination method is widely used because of its short synthesis route and high yield. Pyridine is directly chlorinated at high temperature, and the product varies with the temperature. At 170-270°C, the electrophilic at...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/61C07C41/30C07C43/225B01J20/22B01J20/30
CPCB01J20/22B01J20/30C07B2200/13C07C41/30C07C43/225C07C2603/92C07D213/61
Inventor 黄飞鹤绳新如李二锐周玉娟赵润
Owner ZHEJIANG UNIV
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