تفاعل #2336531

معادلة التفاعل

4-Methylthiophenol

potassium carbonate

DMF

→

isohexane

title compound

المردود 52.0%

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

المردود 52.0%

ظروف التفاعل

المعالجة

1. 1
   أخرىThe mixture was isolated
2. 2
   أخرىto give a yellow solid
3. 3
   أخرىThe solid was purified by flash column chromatography (
4. 4
   غسيلgradient elution

الإجراء التجريبي

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).

المصدر