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Stage #1: With sodium hydroxide; silver(l) oxide In water for 1.5 h; Stage #2: With hydrogenchloride In water
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 2,6-difluoro-4-methylbenzaldehyde (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, 53percent). 1H-NMR (500MHz, d6-DMSO): 613.7 ( br.s, 1H ), 7.02 ( d, 2H, J=9.3 Hz), 2.32 ( s, 3H ).
53%
Stage #1: With sodium hydroxide In hexane; water for 1.5 h; Stage #2: With hydrogenchloride In hexane; water
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 2,6-difluoro-4-methylbenzaldehyde (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, 53percent). 1H-NMR (500MHz, d6-DMSO): 613.7 ( br.s, 1H ), 7.02 ( d, 2H, J=9.3 Hz), 2.32 ( s, 3H ).
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 ).
methyl N-[(10R,14S)-14-amino-10-methyl-9-oxo-8,16-20-diazatricyclo[13.3.1.02'7]nonadeca-1(19),2(7),3,5,15,17-hexaen-5-yl]carbamate dihydrochloride[ No CAS ]
[ 76-05-1 ]
methyl N-[(10R,14S)-14-(2,6-difluoro-4-methylbenzamido)-10-methyl-9-oxo-8,16-diazatricyclo[13.3.1.02,7]nonadeca-1-(19),2(7),3,5,15,17-hexaen-5-yl]carbamate trifluoroacetic acid salt[ No CAS ]
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