反応 #2336531

反応方程式

4-Methylthiophenol

potassium carbonate

DMF

→

isohexane

title compound

収率 52.0%

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

収率 52.0%

反応条件

後処理

1. 1
   その他The mixture was isolated
2. 2
   その他to give a yellow solid
3. 3
   その他The solid was purified by flash column chromatography (
4. 4
   洗浄gradient elution

実験手順

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).

出典