反応 #216796

ord-9db30a027de847a4861373551ca25494

反応条件

温度
0°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他was degassed with argon for 15 minutes at -78° C
  2. 2
    その他The solution was degassed with argon for an additional 5 minutes
  3. 3
    その他The tube was sealed
  4. 4
    温度the mixture was heated to 55° C. for 22 hours

実験手順

A mixture of 1.68 g (5.38 mmol) of 6-bromo-4,4-dibutylthiochroman (Compound 33), 0.28 g (1.5 mmol) of copper (I) iodide and 2.5 g (25 mmol) of triethylamine was degassed with argon for 15 minutes at -78° C. To the suspension was added 1.18 g (71 mmol) of (trimethylsilyl)acetylene and 0.24 g (0.35 mmol) of bis(triphenylphosphine)palladium (II) chloride. The solution was degassed with argon for an additional 5 minutes and the resulting mixture was allowed to warm to 0° C. The tube was sealed and the mixture was heated to 55° C. for 22 hours.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05468879uspto-grants-1995_11