Reaktion #3315

ord-40e5a488e6884a15aae82381ce1c1729

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Einengenconcentrated in vacuo
  2. 2
    Sonstigepartitioned between chloroform and saturated aqueous sodium bicarbonate
  3. 3
    TrocknenThe organic layer was dried over magnesium sulfate
  4. 4
    Filtrationfiltered
  5. 5
    Einengenconcentrated

Vorschrift

To a room temperature solution of 4-chloro-2-methylthio-5-pyrimidinecarboxylate ethyl ester (10.00 g, 43.10 mmol) in 150 mL of tetrahydrofuran was added triethylamine (18.5 mL, 133 mmol) followed by 9 mL of a 70% aqueous solution of ethylamine. The solution was stirred for 30 minutes, then concentrated in vacuo and partitioned between chloroform and saturated aqueous sodium bicarbonate. The organic layer was dried over magnesium sulfate, filtered, and concentrated to provide 9.32 g (90%) of 4-ethylamino-2-methylthio-5-pyrimidinecarboxylate ethyl ester as an oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05733914uspto-grants-1998_03