反应 #3429397
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08552022B2
反应条件: temp:79.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: The 2-methyl-5-nitroisoindolin-1-one (50 mg, 0.26 mmol) was dissolved in EtOH (1.3 ml) with heating, and tin chloride (117 mg, 0.52 mmol) added. The solution was stirred at 79° C. for 2 hours. The mixture was cooled to RT, diluted with 4:1 water:saturated sodium bicarbonate (aq, 100 ml), extracted with EtOAc (3×100 ml), the organics combined, washed with brine, dried over Na2SO4, filtered and the volatiles removed in vacuum. The product was purified by chromatography on SiO2 eluting with 5% MeOH:DCM+1% TEA to give the titled compound. with heating The mixture was cooled to RT saturated sodium bicarbonate (aq, 100 ml), extracted with EtOAc (3×100 ml) washed with brine dried over Na2SO4 filtered the volatiles removed in vacuum The product was purified by chromatography on SiO2 eluting with 5% MeOH
来源 ID: ord-86ee7ff97e5e4cdf86363b1665f13cd9