2,4-Difluoro-5-formylbenzonitrile synthesis
- Product Name:2,4-Difluoro-5-formylbenzonitrile
- CAS Number:633327-10-3
- Molecular formula:C8H3F2NO
- Molecular Weight:167.11
473416-91-0
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Yield:-
Reaction Conditions:
in 1-methyl-pyrrolidin-2-one at 175; for 4 h;
Steps:
81
To a solution of 21.4 g of 5-bromo-2,4-difluoro-benzaldehyde obtained by Production example 80 in 120 mL of N-methyl-2-pyrrolidone, 10.1 g of copper cyanide (I) was added and stirred at 175°C for 4 hours. After allowing the solution to cool, the reaction solution was added with water and diethyl ether, and the impurities were filtered off through Celite. The organic layer was washed successively with water (x3) and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated, and the resulting crude product was purified and separated by silica gel column chromatography (n-hexane:ethyl acetate =9:1), to afford 9.87 g of the title compound as pale yellow crystals.1H-NMR ( 400 MHz, CDCl3) δ 7.14 ( 1H, dd, J = 8.4, 9.6 Hz ), 8.25 ( 1H t, J = 7.2 Hz ), 10.27 ( 1H, s )
References:
EP1510516,2005,A1 Location in patent:Page/Page column 84-85
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329314-68-3
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452-76-6
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