反応 #354353

ord-53c85e6b905d4a6e9054b720b15d8f97

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他contained in a flask
  2. 2
    ろ過The solution was filtered
  3. 3
    その他to remove residual solids
  4. 4
    その他the two-phase filtrate was separated into organic and aqueous phases
  5. 5
    その他The aqueous phase was evaporated to dryness

実験手順

Silver trifluoromethanesulfonate was prepared by slowly adding silver carbonate (13.42 g, 0.052 mol) and small amounts of water (total amount of water was 30 ml) to 14.60 grams (0.097 mol) trifluoromethanesulfonic acid dissolved in 100 ml of 1,1,2-trichloro-1,2,2-trifluoroethane contained in a flask. The solution was filtered to remove residual solids, and the two-phase filtrate was separated into organic and aqueous phases. The aqueous phase was evaporated to dryness to give 15.46 grams of silver salt. The salt was dissolved in 50 ml water; the solution was filtered; and the filtrate was evaporated to dryness. The residual silver trifluoromethanesulfonate was dried at 140° C. in a vacuum oven for four hours. The silver trifluoromethanesulfonate melted at 336°- 338° C. and gave the following elemental analysis: % Ag, 44.24; % C, 4.79; % S, 12.5. Infrared spectral analysis showed major absorption peaks at 8.1, 8.6, 9.8 and 13.05 μ, which are consistent with the indicated structure.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US03940972uspto-grants-1976_03