반응 #2146722

반응 방정식

2-chlorothioxanthone

thiophenol

potassium hydroxide

N,N-dimethylformamide

→

2-(phenylthio)thioxanthone

수율 45.0%

용매

water

반응 조건

후처리

1. 1
   기타react at 130° C. for 9 hours
2. 2
   기타was precipitated
3. 3
   여과This was filtered
4. 4
   세척the residue was washed with water until the pH of the filtrate
5. 5
   기타Then the residue was dried under reduced pressure
6. 6
   기타affording a yellow powdery product
7. 7
   기타The product was purified by column chromatography (eluate:toluene/hexane=1/1:volume ratio)

실험 절차

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)}.

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