PYRIDINE, 5-BROMO-2-(DIFLUOROMETHYL)- synthesis
- Product Name:PYRIDINE, 5-BROMO-2-(DIFLUOROMETHYL)-
- CAS Number:845827-13-6
- Molecular formula:C6H4BrF2N
- Molecular Weight:208
294181-95-6
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845827-13-6
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Yield: 40%
Reaction Conditions:
with potassium fluoride in water;N,N-dimethyl-formamide at 170; for 24 h;Schlenk technique;Inert atmosphere;
Steps:
1
According to the following procedure,5-Bromo-2-difluoromethylpyridine (Compound 4a) was prepared. In the Schlenk tube,The above-obtained 2- (5-bromopyridin-2-yl) -2,2-difluoroacetic acid ethyl ester (compound 3a) (224.1 mg, 0.8 mmol)Potassium fluoride (232.4 mg, 4.0 mmol) and water (72.1 mg, 4.0 mmol) were added and the mixture was stirred at 170 ° C. for 24 hours in a DMF solvent (3.2 mL) under a nitrogen atmosphere. After the reaction, 2,2,2-trifluoroethanol was added as an internal standard, As a result of 19 F-NMR measurement, it was found that 5-bromo-2-difluoromethylpyridine (compound 4a) was produced in a yield of 89%.After that, extraction with diethyl ether, washing with water,And dried over anhydrous sodium sulfate.Anhydrous sodium sulfate was removed by filtration,The filtrate was concentrated under reduced pressure.The residue was purified by silica gel column chromatography (Hexane: diethylether = 20: 1) 5-Bromo-2-difluoromethylpyridine (Compound 4a) (66.8 mg, 0.32 mmol, yield: 40%) was obtained.
References:
GUNMA UNIVERSITY;CENTRAL GLASS COMPANY LIMITED;AMII, HIDEKI;FUJIKAWA, KENICHI;MATSUURA, MAKOTO JP5679855, 2015, B2 Location in patent:Paragraph 0082-0084
31181-90-5
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845827-13-6
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223463-13-6
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1438388-96-5
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845827-13-6
84 suppliers
$30.00/250 mg
223463-13-6
364 suppliers
$5.00/1g
845827-13-6
84 suppliers
$30.00/250 mg