反応 #2030121

ord-c15b1f7e076347e0bacd443ee7230ed3

反応条件

温度
130°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 (25 ml) until an off-white 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 (2.0 g, 7.8 mmol) and p-toluenesulfonic acid methyl ester (2.2 g, 11.7 mmol) was heated in a pressure tube at 130° C. for 2 hours. The mixture was allowed to cool to room temperature, and the resulting mass was triturated with ethyl acetate (25 ml) until an off-white solid separated. The solid was collected by centrifugation, washed with ethyl acetate and dried under vacuum to yield 2.9 g (84%) of Compound 25 whose structure is given below:

出典

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