反応 #334233

ord-5bd3537b61c34a81a5c136dc0cf73388

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度external cooling
  2. 2
    その他the reaction below room temperature
  3. 3
    workup.ADDITIONOnce the addition
  4. 4
    workup.STIRRINGwas stirred at room temperature for 1 h
  5. 5
    洗浄The mixture was then washed with water
  6. 6
    乾燥the organic solution dried (MgSO4)
  7. 7
    その他the solvent evaporated off
  8. 8
    workup.DISTILLATIONthe residue distilled

実験手順

4-Methoxythiophenol (40 mmol) was dissolved in bromochloromethane (0.8 mol) and triethylamine (40 mmol) added dropwise with stirring and external cooling to keep the reaction below room temperature. Once the addition was completed the reaction mixture was stirred at room temperature for 1 h. The mixture was then washed with water, the organic solution dried (MgSO4), the solvent evaporated off and the residue distilled; yield: 3.90 g (52%), b.p. 70° C./0.01 mmHg. The physical data for the title compound are detailed in J. Hayami, N. Tanaka, S. Kurabayashi, Y. Kotani and A. Kaji; Bull.Chem.Soc. (Japan) 44, 3091 (1971).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04705791uspto-grants-1987_11