Reaktion #1064604

ord-d7b4543fe6064b96a7353b5e431836e3

Reaktionsgleichung

OCC[Se]c1ccccc1
2-hydroxyethyl phenyl selenide
O=S(Cl)Cl
thionyl chloride
OCC[Se]c1ccccc1
2-hydroxyethyl phenyl selenide
ClCC[Se]c1ccccc1
2-Chloroethylphenyl Selenide

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction mixture was refluxed for 1 h
  2. 2
    SonstigeThe solvent was evaporated off
  3. 3
    Sonstigethe remaining product transferred to a separatory funnel
  4. 4
    workup.ADDITIONTwenty ml of water was added to the separatory funnel
  5. 5
    SonstigeThe CHCl3 layer was removed from the separatory funnel
  6. 6
    Trocknendried with sodium sulfate
  7. 7
    Sonstigeremoved from the product by rotary evaporation

Vorschrift

One gram of the resulting 2-hydroxyethyl phenyl selenide was dissolved in 15 ml of CH2Cl2. One ml of thionyl chloride was dissolved in 5 ml of CH2Cl2 and was added to the solution of the 2-hydroxyethyl phenyl selenide. The reaction mixture was refluxed for 1 h. The solvent was evaporated off and the remaining product transferred to a separatory funnel using CHCl3. Twenty ml of water was added to the separatory funnel and was made weakly basic with 5% aqueous NaHCO3. The CHCl3 layer was removed from the separatory funnel, dried with sodium sulfate and removed from the product by rotary evaporation and then in vacuo.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05614562uspto-grants-1997_03