反応 #343944

ord-70a8131d2c2242bda19952751b86f54d

溶媒

反応条件

温度
70°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwas charged to a Carius tube under a nitrogen atmosphere
  2. 2
    その他the tube sealed
  3. 3
    温度cooled
  4. 4
    workup.DISTILLATIONthe contents subjected to steam distillation

実験手順

A mixture of 2,2,2-trifluoroethyl bromide (9.8 g), sodium sulphide nonahydrate (14.4 g), sulphur (1.9 g), hexadecyl tributyl phosphonium bromide (1.0 g) and water (18.0 g) was charged to a Carius tube under a nitrogen atmosphere and the tube sealed. The tube was heated to 70° C. for 8 hours, cooled and the contents subjected to steam distillation to give bis-(2,2,2-trifluoroethyl) disulphide as an oil in a yield of 67° C. The product was identified by GC-mass spectroscopy.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05258547uspto-grants-1993_11