反应 #3009699
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06174918B1
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Method 2 (Acid-Promoted Cyclization): A solution of 3a (2.0 g, 0.0009 mol) and Zn (1.0 g) in glacial acetic acid (50 ml) was refluxed for 24 h. A small amount of activated charcoal was added, and the solution was then filtered. The filtrate was poured into a 4-fold excess of H2O. The pH was adjusted to 8 by addition of a solution of NaHCO3, and the resulting solution was then filtered. The recovered precipitate was recrystallized from EtOH to give a dark brown powder (4a). the solution was then filtered The filtrate was poured into a 4-fold excess of H2O The pH was adjusted to 8 by addition of a solution of NaHCO3 the resulting solution was then filtered The recovered precipitate was recrystallized from EtOH
来源 ID: ord-e72ad82953dd457b877a0ba4e6821422