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

In a 1-liter three-necked flask, 46.20g (0.80 mol) of KF was added, followed by 500 mL of N, N-dimethylacetamide, which was warmed to 125 °C and stirred for 30 minutes. The setup was then connected to a distillation unit for micro-vacuum distillation, during which fractions were collected, and the water content was monitored using three separate bottles. Distillation was halted when the water content reached less than 500 ppm. Subsequently, 7g (0.03 mol) of benzyl triethyl ammonium chloride and 100g (0.55 mol) of 2-chloro-5-trifluoromethylpyridine were added to the flask. A condenser was connected, and the mixture was warmed to 135 °C and stirred for 10 hours. Gas chromatography was used to monitor the reaction; the reaction was stopped when the content of 2-chloro-5-trifluoromethylpyridine in the reaction solution was less than 1%. The reaction solution was directly distilled under reduced pressure to collect the fraction at 40-45 °C / 11 mmHg, yielding 87.80g of 2-fluoro-5-trifluoromethylpyridine with a purity of 98.95% (GC) and a yield of 95.56%.

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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