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Method for synthesizing 2-chloropyridine

A chloropyridine and pyridine technology, applied in the field of 2-chloropyridine synthesis, can solve the problems of low single-pass yield, many by-products, and high process requirements, and achieve the effect of safe and reliable process production

Inactive Publication Date: 2016-06-15
ANHUI COSTAR BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0016] Route 4 has relatively high process requirements, more by-products and low single-pass yield

Method used

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  • Method for synthesizing 2-chloropyridine
  • Method for synthesizing 2-chloropyridine
  • Method for synthesizing 2-chloropyridine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 79g of pyridine and 170g of dichloromethane into a 500mL container, stir for 15min, then add 95g of fluorine acetate dropwise at a rate of 3g / min for 30min, and react at 20°C for 4 hours; transfer the reaction mixture to 500mL In the container, carry out vacuum distillation under the conditions of temperature 70°C and vacuum degree 0.07Mpa. After no liquid is evaporated, the remaining material is 2-chloropyridine. The content of 2-chloropyridine was detected to be 94.5%, and the yield was 80.2%.

Embodiment 2

[0031] Add 79g of pyridine and 170g of dichloromethane into a 500mL container, stir for 15min, then dropwise add 100g of fluorine acetate at a rate of 4g / min, dropwise for 30min, and react at 20°C for 4 hours; transfer the reaction mixture to 500mL In the container, carry out vacuum distillation under the conditions of temperature 60°C and vacuum degree 0.07Mpa. After no liquid is evaporated, the remaining material is 2-chloropyridine. The content of 2-chloropyridine was detected to be 94.8%, and the yield was 80.8%.

Embodiment 3

[0033] Add 79g of pyridine and 170g of dichloromethane into a 500mL container, stir for 15min, then add 105g of fluorine acetate dropwise at a rate of 4g / min for 30min, and react at 20°C for 4 hours; transfer the reaction mixture to 500mL In the container, carry out vacuum distillation under the conditions of temperature 50°C and vacuum degree 0.07Mpa. After no liquid is evaporated, the remaining material is 2-chloropyridine. The content of 2-chloropyridine was detected to be 94.7%, and the yield was 81.3%.

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Abstract

The invention discloses a method for synthesizing 2-chloropyridine. The steps of the method are to add pyridine and solvent into a 500mL container, control the pressure at normal pressure, stir for 10-20min, then add fluorine acetate dropwise, and control the temperature not to exceed 30°C; move the reaction mixture to a 500mL container, The temperature is raised to 50°C-70°C, vacuum distillation is carried out under the conditions of vacuum degree 0.07-0.09MPa, and after no liquid is evaporated, the remaining material is 2-chloropyridine. The chlorination of the inventive method does not need highly toxic substances such as chlorine gas, phosphorus trichloride, phosphorus pentachloride, phosphorus oxychloride and phosgene as the chlorination reagent, but uses dichloromethane as the chlorination reagent. It is safe and reliable; the reaction is carried out under normal temperature and pressure, and the yield of 2-chloropyridine reaches 80%.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a synthesis method of 2-chloropyridine. Background technique [0002] 2-Chloropyridine is an important chemical intermediate, mainly used in the synthesis of medicines and pesticides, some of which have been widely used in daily chemicals and crop protection, and the market prospect is promising. In medicine, 2-chloropyridine can produce antihistamine——pheniramine (1) and antiarrhythmic drug——dasupine (2); in daily chemical products, 2-chloropyridine can produce a Fungicide—pythione zinc salt (3); in terms of pesticides, forchlorfenuron (4) can be produced, which is a brand-new plant growth regulator with high activity, low toxicity, and broad spectrum. The splitting activity is 10-100 times that of kinetin and zeatin. Applying before flowering can induce parthenocarpy to form seedless fruit and improve the fruit setting rate of crops. When applied at flowering or aft...

Claims

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Application Information

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IPC IPC(8): C07D213/61
CPCC07D213/61
Inventor 韦永飞梁锡臣赵广福吴海峡孔军军史玉龙
Owner ANHUI COSTAR BIOCHEM CO LTD
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