반응 #2336531

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4-Methylthiophenol

potassium carbonate

DMF

→

isohexane

title compound

수율 52.0%

3,6-Bis(4′-methylphenylthio) phthalonitrile

수율 52.0%

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후처리

1. 1
   기타The mixture was isolated
2. 2
   기타to give a yellow solid
3. 3
   기타The solid was purified by flash column chromatography (
4. 4
   세척gradient elution

실험 절차

4-Methylthiophenol (3.41 g, 27.5 mmol), potassium carbonate (3.80 g, 27.5 mmol) and ditosylated dicyanohydroquinone (i.e. product A) (5.00 g, 10.7 mmol) in DMF (40 mL) were reacted as described above. The mixture was isolated as described above to give a yellow solid. The solid was purified by flash column chromatography (gradient elution: 5%-10%-30% ethyl acetate:isohexane, finally dichloromethane) to give the title compound as a yellow solid (2.07 g, 52%). [Found: C, 69.9%; H, 4.4%; N, 7.3%; S, 16.9%; C22H16N2S2 requires C, 70.9%, H, 4.3%, N, 7.5%, S, 17.2%]; MS (EI+) 372 (M+, 100%), 357 (M-CH3, 5%), 123 (CH3C6H4S, 15), 91 (CH3C6H4, 15).

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