ChemicalBook CAS DataBase List 2-Chloro-4-cyanopyridine

2-Chloro-4-cyanopyridine synthesis

5synthesis methods

Product Name:2-Chloro-4-cyanopyridine
CAS Number:33252-30-1
Molecular formula:C6H3ClN2
Molecular Weight:138.55

14906-59-3

33252-30-1

The general procedure for the synthesis of 2-chloro-4-cyanopyridine from 4-cyanopyridine N-oxide was as follows: 120 g of 4-cyanopyridine-N-oxide, 360 mL of 1,2-dichloroethane, and 183.6 g of phosphorochloridic acid were added sequentially in a 1000 mL three-necked reaction flask. After the reaction system was cooled to -2±2°C, 151.5 g of triethylamine was added slowly dropwise for a controlled dropwise time of 2 hours. After the dropwise addition, the reaction was continued at the same temperature with stirring for 2 hours. Upon completion of the reaction, the reaction solution was concentrated by reduced pressure distillation until no fractions flowed out. 240 mL of water was added to the concentrated solution and a large amount of solid was precipitated after thorough stirring. The solid was collected by filtration and the filter cake was washed with appropriate amount of water to obtain 117.5 g of white solid product 2-chloro-4-cyanopyridine.

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33252-30-1
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Yield:33252-30-1 117.5 g

Reaction Conditions:

with triethylamine;trichlorophosphate in 1,2-dichloro-ethane; for 4 h;

Steps:

In a 1000ml reaction flask,Add 4-cyanopyridine-N-oxide 120g,1,2-dichloroethane 360ml,Phosphorus oxychloride 183.6g,Cool the reaction system to -2±2°C,Triethylamine 151.5g was added dropwise.The dripping time is 2h. After the dripping is completed, the incubation time is 2h. After the reaction is completed,The reaction solution was concentrated until no more fractions flowed out.Add 240ml water,Stirring,There are a lot of solids out,Suction filtrationThe filter cake is rinsed with water.dry,117.5g of white solidThat is 2-chloro-4-cyanopyridine.

References:

CN104945383,2017,B Location in patent:Paragraph 0031; 0035; 0036

14906-59-3
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$27.00/5g