تفاعل #2146722

معادلة التفاعل

2-chlorothioxanthone

thiophenol

potassium hydroxide

N,N-dimethylformamide

→

2-(phenylthio)thioxanthone

المردود 45.0%

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   أخرىreact at 130° C. for 9 hours
2. 2
   أخرىwas precipitated
3. 3
   ترشيحThis was filtered
4. 4
   غسيلthe residue was washed with water until the pH of the filtrate
5. 5
   أخرىThen the residue was dried under reduced pressure
6. 6
   أخرىaffording a yellow powdery product
7. 7
   أخرىThe product was purified by column chromatography (eluate:toluene/hexane=1/1:volume ratio)

الإجراء التجريبي

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)}.

المصدر