反応 #339927

ord-055415cca59945b8bceb21d685114554

反応条件

温度
70°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度to cool to room temperature
  2. 2
    その他partitioned between AcOEt
  3. 3
    その他After separation
  4. 4
    洗浄the organic layer was washed with water and brine
  5. 5
    乾燥dried over anhydrous Na2SO4
  6. 6
    ろ過filtered
  7. 7
    濃縮concentrated

実験手順

Ammonia was bubbled for 5 min in a solution of 2,4-dichloro-6-piperidin-1-yl-[1,3,5]triazine (500 mg, 2.15 mmol) in dry 1,4-dioxane (20 mL). The solution was heated at 70° C. for 16 h in a sealed tube. The reaction mixture was allowed to cool to room temperature, and partitioned between AcOEt and a solution of sat. NH4Cl. After separation, the organic layer was washed with water and brine, dried over anhydrous Na2SO4, filtered and concentrated to afford the title compound 221 (453 mg, 2.12 mmol, 98% yield). LRMS: [MH]=214.1.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07868204B2uspto-grants-2011_01