反応 #162607

ord-4efd0c7fad3648f0a27c02c0fdeebb29

反応条件

温度
100°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他In a 25 mL round-bottomed flask was placed
  2. 2
    温度The mixture was cool to room temperature
  3. 3
    workup.ADDITIONpoured on ice
  4. 4
    抽出extracted with dichloromethane
  5. 5
    乾燥The organic phase was dried over MgSO4
  6. 6
    ろ過filtered
  7. 7
    濃縮concentrated

実験手順

In a 25 mL round-bottomed flask was placed 4,6-di(8-oxa-3-azabicyclo[3.2.1]octan-3-yl)pyrimidin-2-ol (27), 12 mg, 0.038 mmol) in POCl3 (3 ml) to give a yellow solution. The mixture was stirred at 100° C. for 4 h. The mixture was cool to room temperature, poured on ice, and extracted with dichloromethane. The organic phase was dried over MgSO4, filtered and concentrated to give the title compound as a white crystalline solid (12 mg, 93%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08835429B2uspto-grants-2014_09