Reaktion #460631

ord-423b25bb2aec422eb09329449dba1a48

Reaktionsgleichung

c1cncnc1
pyrimidine
C[O-].[Na+]
sodium methoxide
Cc1nc(Cl)c(Cl)c(Cl)n1
2-methyl-4,5,6-trichloropyrimidine
O
Water
COc1nc(C)nc(Cl)c1Cl
4,5-Dichloro-6-methoxy-2-methylpyrimidine

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas added slowly
  2. 2
    Extraktionthe resulting mixture was extracted with methylene chloride
  3. 3
    SonstigeRemoval of the solvent and other volatiles from the
  4. 4
    Extraktionextract by evaporation under reduced pressure
  5. 5
    workup.WAITleft the title compound as a white powder melting at 77°-78° C.

Vorschrift

A solution containing 38 g (0.17 mol) of 2-methyl-4,5,6-trichloropyrimidine in 200 ml of methanol was cooled in an ice bath to 10`-15° C. and sodium methoxide as a 25 percent solution in methanol was added slowly with stirring until the starting pyrimidine could no longer be detected by GLC analysis. Water was then added and the resulting mixture was extracted with methylene chloride. Removal of the solvent and other volatiles from the extract by evaporation under reduced pressure left the title compound as a white powder melting at 77°-78° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05163995uspto-grants-1992_11