反応 #2336532

反応方程式

Water

Thiophenol

potassium carbonate

DMF

→

title compound

収率 52.0%

3,6-Bis(phenylthio) phthalonitrile

収率 52.0%

反応条件

後処理

1. 1
   ろ過then filtered
2. 2
   その他The filter cake was purified by flash column chromatography (gradient elution 10%-30% ethyl acetate:isohexane)

実験手順

Thiophenol (11.75 g, 107 mmol), potassium carbonate (14.74 g, 107 mmol) and ditosylated dicyanohydroquinone (25.00 g, 53.0 mmol) in DMF (80 mL) were reacted as described above. Water (100 mL) was added and the mixture stirred for 1 hour then filtered. The filter cake was purified by flash column chromatography (gradient elution 10%-30% ethyl acetate:isohexane) to give the title compound as a yellow solid (5.53 g, 16.1 mmol, 52%). [Found: C, 69.6%; H, 3.5%; N, 8.2%; S, 18.3%; C20H12N2S2 requires C, 69.8%; H, 3.5%; N, 8.1%; S, 18.6%]; MS (EI+) 344 (M+, 100%).

出典