反応 #491648

ord-1b65c9c7b5ed4425858e8e2f0f795732

反応条件

温度
72.5°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwas added in a single portion
  2. 2
    温度to cool to room temperature
  3. 3
    その他the title compound was removed by filtration
  4. 4
    洗浄washed with water
  5. 5
    その他dried under vacuum

実験手順

To a solution of 8-oxa-3-azabicyclo[3.2.1]octane hydrochloride (0.49 g, 3.3 mmol) in water (18 mL) was added a suspension of tert-butyl 4-(4,6-dichloro-1,3,5-triazin-2-yl)piperazine-1-carboxylate (1.0 g, 3.0 mmol) in acetone (about 10 mL). The suspension was stirred magnetically while solid sodium carbonate (0.70 g, 6.6 mmol) was added in a single portion. The mixture was stirred for two hours while heating in a 70-75° C. in an oil bath. After allowing the mixture to cool to room temperature, the title compound was removed by filtration, washed with water, and dried under vacuum.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08748421B2uspto-grants-2014_06