Reaktion #44525

ord-ee4c67b25ee64efdb3c0893c80b0defa

Reaktionsgleichung

CSc1nccc(Cl)n1
4-chloro-2-methylsulfanylpyrimidine
N
ammonia
CSc1nccc(N)n1
2-(methylsulfanyl)-4-pyrimidinamine

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooled
  2. 2
    Einengenconcentrated
  3. 3
    workup.ADDITIONtreated with water
  4. 4
    Extraktionextracted with ethyl acetate
  5. 5
    WaschenThe extract was washed with brine
  6. 6
    Trocknendried over anhydrous sodium sulfate
  7. 7
    Einengenconcentrated
  8. 8
    SonstigeThe concentrate was triturated with ethyl ether
  9. 9
    Filtrationfiltered

Vorschrift

A mixture of 4-chloro-2-methylsulfanylpyrimidine (8 g) and 7N ammonia in methanol (100 mL) at 100° C. was stirred for 2 days in a sealed tube, cooled, concentrated, treated with water, and extracted with ethyl acetate. The extract was washed with brine, dried over anhydrous sodium sulfate, and concentrated. The concentrate was triturated with ethyl ether and filtered. 1H NMR (300 MHz, CDCl3) δ 8.06 (d, 1H), 6.12 (d, 1H), 4.83 (s, 2H), 2.51 (s, 3H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07737159B2uspto-grants-2010_06