反应 #1753713
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06239159B1
反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: TOSMIC (1.5 g, 7.7 mmol) was added to a solution of dimethyl fumarate (1 g, 6.9 mmol) and sodium hydride (60%, 0.59, 12.5 mmol) in dry DMF (25 ml) at 0° C., and the solution stirred at 0° C. for 15 minutes. The reaction was poured onto ice-water and the product filtered and recrystallised from aqueous ethanol. 0.61 g, 48%. 1H-n.m.r. (DMSO-d6) δ (ppm) 3.68 (6H, s, 2×CH3), 7.39 (2H, s, 2×CH), 11.81 (1H, s, NH). The reaction was poured onto ice-water the product filtered recrystallised from aqueous ethanol
来源 ID: ord-a009546adac7428ebb42b87d9cf41f2e