反応 #2146723

反応方程式

hydrogen peroxide

2-(phenylthio)thioxanthone

acetonitrile

sulfuric acid

→

2-[(phenyl)sulfinyl]thioxanthone

収率 83.0%

溶媒

water

反応条件

後処理

1. 1
   温度Subsequently, the reaction solution was cooled to room temperature (about 25° C.)
2. 2
   その他was precipitated
3. 3
   ろ過This was filtered
4. 4
   洗浄the residue was washed with water until the pH of the filtrate
5. 5
   その他Then the residue was dried under reduced pressure
6. 6
   その他affording a yellow powdery product
7. 7
   その他The product was purified by column chromatography (eluate: ethyl acetate/toluene=⅓:volume ratio)

実験手順

While 11.2 parts of 2-(phenylthio)thioxanthone synthesized in Production Example 1, 215 parts of acetonitrile, and 0.02 parts of sulfuric acid were stirred at 40° C., 4.0 parts of a 30% aqueous hydrogen peroxide solution was dropped thereto slowly and then a reaction was performed at 40 to 45° C. for 14 hours. Subsequently, 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: ethyl acetate/toluene=⅓:volume ratio) to afford 2-[(phenyl)sulfinyl]thioxanthone in a yield of 83%. The product was identified by 1H-NMR {d6-dimethyl sulfoxide, δ (ppm) 8.75 (1H, s), 8.45 (1H, d), 8.01 (2H, d), 7.75-7.85 (4H, m), 7.53-7.62 (4H, m)}.

出典