ChemicalBook CAS DataBase List 2-Fluoro-5-trifluoromethylpyridine

2-Fluoro-5-trifluoromethylpyridine synthesis

7synthesis methods

Product Name:2-Fluoro-5-trifluoromethylpyridine
CAS Number:69045-82-5
Molecular formula:C6H3F4N
Molecular Weight:165.09

52334-81-3
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69045-82-5
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$5.00/1g

Yield:69045-82-5 95.56%

Reaction Conditions:

with potassium fluoride;N-benzyl-N,N,N-triethylammonium chloride in N,N-dimethyl acetamide at 135; for 10 h;Solvent;Reagent/catalyst;Temperature;

Steps:

1 Example 1:

1, to 1L three-necked flask was added KF46.20g (0.80mol),500 mL of N, N-dimethylacetamide, warmed to 125 ° C.,Stir for 30 minutes,Connected to the distillation unit,Micro-vacuum distillation, collecting fractions, tracking three bottles of water content, water <500ppm, stop distillation, stand-by.
2, to three bottles of benzyl triethyl ammonium chloride 7g (0.03mol),100 g (0.55 mol) of 2-chloro-5-trifluoromethylpyridine.Connect the condenser, warmed to 135 ,Stirring, incubated for 10 hours.Gas chromatography followed the reaction, when the reaction solution 2-chloro-5-trifluoromethylpyridine content <1%, stop the reaction.The reaction solution was directly distilled under reduced pressure to collect 40-45 ° C / 11 mmHg fraction,87.80 g of 2-fluoro-5-trifluoromethylpyridine was obtained,Purity 98.95% (GC), yield 95.56%.

References:

CN106946769,2017,A Location in patent:Paragraph 0028; 0029; 0030; 0031; 0032; 0033-0045