Reaktion #595343

ord-206771c8f13e40dd8874837b02bbecb1

Reaktionsgleichung

CCc1oc(-c2ccc(Cl)cc2)[n+]([O-])c1C
compound
CCc1oc(-c2ccc(Cl)cc2)[n+]([O-])c1C
2-(4-Chlorophenyl)-5-ethyl-4-methyl-1,3-oxazole 3-oxide
O=P(Cl)(Cl)Cl
phosphoryl chloride
N
ammonia
CCc1oc(-c2ccc(Cl)cc2)nc1CCl
4-(Chloromethyl)-2-(4-chlorophenyl)-5-ethyl-1,3-oxazole

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture is heated
  2. 2
    Temperaturto reflux
  3. 3
    ExtraktionThe reaction mixture is extracted three times with in each case 20 ml of ethyl acetate
  4. 4
    SonstigeThe solvent is removed on a rotary evaporator
  5. 5
    Sonstigethe residue is dried in a vacuum
  6. 6
    Sonstigedrying cabinet
  7. 7
    SonstigeThe product is used without further purification in the subsequent reactions

Vorschrift

1.00 g (4.21 mmol) of the compound from Example 29A are dissolved in 15 ml of chloroform, and 1.4 ml (15.15 mmol) of phosphoryl chloride are added carefully. The mixture is heated to reflux and stirred at this temperature for 30 min. The mixture is then cooled to 0° C. and made slightly basic using ammonia. The reaction mixture is extracted three times with in each case 20 ml of ethyl acetate. The solvent is removed on a rotary evaporator and the residue is dried in a vacuum drying cabinet. The product is used without further purification in the subsequent reactions.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09095582B2uspto-grants-2015_08