Reaktion #979433

ord-b772262f50cf4758a8c36b32131eb340

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturto cool down over night
  2. 2
    ExtraktionThe reaction mixture was extracted with three portions of sodium bicarbonate solution
  3. 3
    Extraktionextracted three times with ethyl acetate
  4. 4
    ExtraktionThe organic extract
  5. 5
    Sonstigewas dried
  6. 6
    Sonstigeevaporated

Vorschrift

To a solution of 28.46 g (0.182 mol) 1,3-dimethyl-pyrimidine-2,4,6-trione and 1.81 g (1.57 mmol) tetrakis-(triphenylphosphine)-palladium in 600 ml dichloromethane was added dropwise a solution of 17.70 g (60.75 mmol) 1-[2-(4-allyloxy-phenylmethanesulfinyl)-ethyl]-1H-[1,2,3]triazole and stirring was continued for 6 hours at 45° C. It was allowed to cool down over night. The reaction mixture was extracted with three portions of sodium bicarbonate solution, then the aqueous phase was adjusted to pH 1 and extracted three times with ethyl acetate. The organic extract was dried and evaporated to yield 12.6 g (83%) 4-(2[1,2,3] triazol-1-yl-ethanesulfinylmethyl)-phenol as white solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07005526B2uspto-grants-2006_02