* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Silver oxide (43.8 g, 0.189mol) was placed in a flask along with water (20OmL) and sodium hydroxide (33.7g, 0.842mol). To it was added <strong>[1201597-22-9]2,6-difluoro-4-methylbenzaldehyde</strong> (29.23 g, 0.187mol) in small portions over a 30min period. After a vigorous exothermic reaction, the color of the reaction mixture changed from black to gray. The resulting thick suspension was stirred for 1 hr and then filtered through a Buchner funnel. The filtrate was acidified to pH 2 with concentrated HCl to give a suspension. The precipitate was collected by suction filtration, dissolved in ether, dried over anhydrous Na2SO4, filtered and concentrated to give white solid (17.0 g, 53%). 1H-NMR (500MHz, d6-DMSO): 613.7 ( br.s, 1H ), 7.02 ( d, 2H, J=9.3 Hz), 2.32 ( s, 3H ).
53%
Step C: 2,6-difluoro-4-methylbenzoic acid Silver oxide (43.8 g, 0.189mol) was placed in a flask along with water (20OmL) and sodium hydroxide (33.7g, 0.842mol). To it was added <strong>[1201597-22-9]2,6-difluoro-4-methylbenzaldehyde</strong> (29.23 g, 0.187mol) in small portions over a 30min period. After a vigorous exothermic reaction, the color of the reaction mixture changed from black to gray. Resulting thick suspension was stirred for 1 hr, filtered through a Buchner funnel. The filtrate was acidified to pH 2 with concentrated HCl to give a suspension. The precipitate was collected by suction filtration, dissolved in ether and dried over anhydrous Na2SO4, filtered and concentrated to give white solid (17.0 g, 53%). 1H-NMR (500MHz, d6-DMSO): 613.7 ( br.s, 1H ), 7.02 ( d, 2H, J=9.3 Hz), 2.32 ( s, 3H ).
Chemistry
Pharmaceutical Intermediates
Inhibitors/Agonists
Material Science
For Research Only
120K+ Compounds
Competitive Price
1-2 Day Shipping
