Reaktion #83374

Reaktionsgleichung

3-Chloro-6-phenylpyridazine

4-aminothiophenol

potassium carbonate

→

3-(4-aminophenylthio)-6-phenylpyridazine

Ausbeute 83.0%

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationThe reaction was filtered
2. 2
   Einengenconcentrated
3. 3
   workup.ADDITIONethyl acetate added
4. 4
   Waschenwashed with water
5. 5
   Trocknendried over sodium sulfate
6. 6
   EinengenThe solution was concentrated
7. 7
   Sonstigethe product purified by HPLC over silica gel
8. 8
   Wascheneluted with 50% ethyl acetate/hexane

Vorschrift

3-Chloro-6-phenylpyridazine (0.026 moles, 5.0 g), 4-aminothiophenol (0.026 moles, 3.3 g) and potassium carbonate (0.026 moles, 3.6 g) were stirred in 250 ml ethanol for 3 days. The reaction was filtered, concentrated, ethyl acetate added, washed with water and dried over sodium sulfate. The solution was concentrated and the product purified by HPLC over silica gel eluted with 50% ethyl acetate/hexane to yield 3-(4-aminophenylthio)-6-phenylpyridazine 6.0 g, 83%. Mass Spec (FD) 279. Calculated for C16H13N3S: C, 68.79; H, 4.69; N, 15.04. Found: C, 68.87; H, 4.43 N, 15.31.

Quelle