反応 #1064120

ord-c28af50d0d804a7c87b400aa7669d65d

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他is held at 70°-80° C.
  2. 2
    workup.ADDITIONis added dropwise
  3. 3
    その他a positive reaction
  4. 4
    温度The violet-red precipitate is cooled
  5. 5
    その他recrystallized from ethanol or acetone
  6. 6
    その他to yield 8

実験手順

To a solution of 16 g 2,4-diamino-6-benzyloxy-pyrimidine (7) in 250 mL of warm 30% acetic acid is added a solution of 7 g sodium nitrite in 25 mL H2O. The sodium nitrite solution is held at 70°-80° C. and is added dropwise while being stirred continuously. The sodium nitrite solution is added until potassium-iodate starch paper shows a positive reaction. The violet-red precipitate is cooled, suctioned off and then recrystallized from ethanol or acetone to yield 8.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05612468uspto-grants-1997_03