反応 #465673

ord-4e7a78235a094b98b9fdb25f1cc51634

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The reaction mixture was heated
  2. 2
    温度maintained at this temperature for 30 minutes
  3. 3
    その他to precipitate
  4. 4
    ろ過The reaction mixture was filtered
  5. 5
    その他to remove the inorganic salts
  6. 6
    その他the resulting solution placed on a rotary evaporator
  7. 7
    その他to remove solvents
  8. 8
    その他The product crystallized

実験手順

In a 100 mL Erlenmeyer flask were combined 10 g (0.05 mol) phenacyl bromide, 12.93 g (0.05 mol) sodium hexafluoroantimonate, 15 g (0.05 mol) methyl octadecyl sulfide and 40 mL methyl ethyl ketone (2-butanone). The reaction mixture was heated to boiling and maintained at this temperature for 30 minutes. During this time, sodium bromide was observed to precipitate. The reaction mixture was filtered to remove the inorganic salts and the resulting solution placed on a rotary evaporator to remove solvents. The product crystallized to give the desired salt, m.p. 80-82° C. Recrystallization from isopropanol gave a very light tan salt with a melting point of 79-80° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06031014uspto-grants-2000_02