反応 #2030122

ord-2cdc599eee1f4bc192502358e3e72575

反応条件

温度
160°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the resulting mass was triturated with ethyl acetate (40 ml) until a pink solid
  3. 3
    その他separated
  4. 4
    その他The solid was collected by centrifugation
  5. 5
    洗浄washed with ethyl acetate
  6. 6
    その他dried under vacuum

実験手順

A mixture of Compound 24 (2.55 g, 10.0 mmol) from step (a) of Example 27 and 1-4-butane sultone (2.98 g, 21.9 mmol) was heated in a pressure tube at 160° C. for 17 hours. The mixture was allowed to cool to room temperature, and the resulting mass was triturated with ethyl acetate (40 ml) until a pink solid separated. The solid was collected by centrifugation, washed with ethyl acetate and dried under vacuum to yield 3.58 g (92%) of Compound 26 with the structure:

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08389729B2uspto-grants-2013_03