反応 #216790

ord-8659ecf51d56489ba0aa8c1e264f4b54

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 heated to 55° C. for 15 hours

実験手順

A mixture of 1.96 g (6.90 mmol) of 6-bromo-4,4-diethylthiochroman (Compound 25), 0.11 g (0.59 mmol) of copper (I) iodide and 4.36 g (4.31 mmol) of triethylamine was degassed with argon for 15 minutes at -78° C. To the suspension was added 6.95 g (71 mmol) of (trimethylsilyl)acetylene then 0.41 g (58 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 heated to 55° C. for 15 hours.

出典

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