反応 #1118271

ord-ecfdebccf53949eabe3eb82d41824461

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度to cool
  2. 2
    ろ過The resulting precipitate was collected by filtration
  3. 3
    洗浄washed with water and ethanol

実験手順

A solution of 4,5-diamino-1-methylbenzotriazole (1.2 g, 7.4 mmol) and oxalic acid dihydrate (1.2 g, 9.6 mmol) in 40 ml of 4M hydrochloric acid was refluxed on an oil bath for 2 h and allowed to cool. The resulting precipitate was collected by filtration and washed with water and ethanol to give 1.46 g (91%) of the title compound; m.p. >300° C.; IR (KBr): 1700 cm-1 ; 1H-NMR (DMSO-d6): 4.32 (s, 3H, CH3), 7.33 (d, J=9 Hz), 1H, ArH), 7.55 (d, J=9 Hz, 1H, ArH), 12.03 (broad s, 1H, OH), 12.67 (broad s, 1H, OH).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05109001uspto-grants-1992_04