Reaktion #2146722

Reaktionsgleichung

2-chlorothioxanthone

thiophenol

potassium hydroxide

N,N-dimethylformamide

→

2-(phenylthio)thioxanthone

Ausbeute 45.0%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigereact at 130° C. for 9 hours
2. 2
   Sonstigewas precipitated
3. 3
   FiltrationThis was filtered
4. 4
   Waschenthe residue was washed with water until the pH of the filtrate
5. 5
   SonstigeThen the residue was dried under reduced pressure
6. 6
   Sonstigeaffording a yellow powdery product
7. 7
   SonstigeThe product was purified by column chromatography (eluate:toluene/hexane=1/1:volume ratio)

Vorschrift

After mixing 11.0 parts of 2-chlorothioxanthone, 4.9 parts of thiophenol, 2.5 parts of potassium hydroxide, and 162 parts of N,N-dimethylformamide uniformly and then making them react at 130° C. for 9 hours, the reaction solution was cooled to room temperature (about 25° C.) and then was poured into 200 parts of distilled water, so that the product was precipitated. This was filtered and the residue was washed with water until the pH of the filtrate became neutral. Then the residue was dried under reduced pressure, affording a yellow powdery product. The product was purified by column chromatography (eluate:toluene/hexane=1/1:volume ratio) to afford 2-(phenylthio)thioxanthone in a yield of 45%. The product was identified by 1H-NMR {d6-dimethyl sulfoxide, δ (ppm) 8.43 (1H, d), 8.25 (1H, s), 7.75-7.90 (3H, m), 7.66 (1H, d), 7.60 (1H, t), 7.42-7.46 (5H, m)}.

Quelle