反応 #2146722

反応方程式

2-chlorothioxanthone

thiophenol

potassium hydroxide

N,N-dimethylformamide

→

2-(phenylthio)thioxanthone

収率 45.0%

溶媒

water

反応条件

後処理

1. 1
   その他react at 130° C. for 9 hours
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:toluene/hexane=1/1:volume ratio)

実験手順

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)}.

出典