反応 #595684

ord-022d721bc28c4b269ffac6dd6c501d38

反応条件

温度
80°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The reaction was cooled to room temperature
  2. 2
    濃縮concentrated by rotary evaporation
  3. 3
    抽出The product was extracted with EtOAc (3×10 mL)
  4. 4
    乾燥The combined organic extracts were dried over MgSO4
  5. 5
    濃縮concentrated

実験手順

4-Fluorobenzyl bromide (23 μL, 0.19 mmol) and potassium carbonate (100 mg, 0.78 mmol) were added to a solution of N-ethylcarbamate-5-hydroxy-6-chloro-8-methyl-1,2,3,3a,8,8a-hexahydroindeno[1,2-c]pyrrole (from Example 5, Step A) (46 mg, 0.16 mmol) in acetonitrile (3 mL), and stirred overnight at 80° C. The reaction was cooled to room temperature, concentrated by rotary evaporation and taken up in H2O (5 mL). The product was extracted with EtOAc (3×10 mL). The combined organic extracts were dried over MgSO4 and concentrated to afford the subtitle compound, which was used without further purification. MS calculated for C22H23ClFNO3+H: 404, observed: 404.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09096520B2uspto-grants-2015_08