Reaktion #8698

ord-50ab374672784712afdda58eb7ef9ef4

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeBulk of the solvent was evaporated before it
  2. 2
    workup.ADDITIONwas diluted with diethyl ether (50 ml)
  3. 3
    SonstigeThe precipitate that formed
  4. 4
    Sonstigewas collected
  5. 5
    Waschenwashed with diethyl ether (100 ml)
  6. 6
    Sonstigedried

Vorschrift

A solution of 4,6-dichloro-5-(2-methoxyphenoxy)-2-(4-pyridyl)-pyrimidine (2 g) and 2-phenyl-ethanesulfonic acid amide potassium salt (2.82 g, Referential Example 1e) in DMF (50 ml) was stirred at rt for 16 h. Bulk of the solvent was evaporated before it was diluted with diethyl ether (50 ml). The mixture was acidified with 10% aq. citric acid. The precipitate that formed was collected, washed with diethyl ether (100 ml) and dried to give 2-phenyl-ethanesulfonic acid [6-chloro-5-(2-methoxy-phenoxy)-2-pyridin-4-yl-pyrimidin-4-yl]-amide (2.23 g) as a beige powder. LC-MS: tR=4.93 min, [M+1]+=497.22, [M−1]−=494.96.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07091201B2uspto-grants-2006_08