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酰胺甲醛制备腈也是个人名反应?von Braun酰胺甲醛反应

2023-02-25 12:16:21

led. After cooling the mixtureovernight, a crude was obtained by filtration. Additional material was obtained by recovery from the mother liquid. The combined solids were stirred in MeOH (0.7L) for between 1 and 3 h, filtered and dried in a vacuum oven between 50~80 degC.at 25 Torr with a nitrogen bleed to afford 339 g of 22 (90percent theory).

At ice-water bath, oxalyl chloride (0.345 ml) wasadded dropwise to a solution of 1.0 g of ethyl1-{4-[2-(t-butylaminocarbonyl)phenyl]phenyl}methyl-4-(1-hydroxy-1-methylethyl)-2-propylimidazole-5-carboxylate in 10 ml of methylene chloride. The mixture was stirred at the sametemperature for 2 hours. The reactionmixture was diluted with an aqueous solution of sodium hydrogencarbonate andethyl acetate, and the ethyl acetate layer was separated, dried over anhydrousmagnesium sulfate and concentrated by evaporation under reduced pressure. The residue was purified by silica gel columnchromatography, using 1:1 EtOAc/hex (v/v) as the eluent, to give 0.69 g of thetitle compound as crystals.

参考

彼此之间关反应会

Ritter反应会

Beckmann醛反应会

Schmidt醛

苯甲酸溶解制备衍生物

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