反应 #2942536
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09115136B2
反应条件: temp:110.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of 4′-{[7-butyl-5-oxo-4-(4-oxocyclohexyl)-4,5-dihydro[1,2,4]triazolo[1,5-a]pyrimidin-6-yl]methyl}biphenyl-2-carbonitrile (1 g), 2,3-dimethylpropane-1,3-diol (0.56 g), p-toluenesulfonic acid monohydrate (0.036 g) and toluene (30 mL) was subjected to an azeotropic dehydration reaction by stirring at 110° C. for 3 hr in a reaction vessel equipped with a Dean-stark trap. The reaction mixture was concentrated under reduced pressure, and the obtained residue was purified by silica gel column chromatography to give the title compound as a colorless solid (1.2 g, 100%). was subjected to an azeotropic dehydration reaction equipped with a Dean-stark trap The reaction mixture was concentrated under reduced pressure the obtained residue was purified by silica gel column chromatography
来源 ID: ord-29ab129aac2c4285a14c0d35ec3f3e36