反応 #49733

反応方程式

Thiophenol

2-nitro-4-trifluoromethylbenzonitrile

thiophenol

potassium carbonate

Water

→

2-(phenylsulphenyl)-4-trifluoromethylbenzonitrile

収率 85.2%

溶媒

acetonitrile

反応条件

後処理

1. 1
   温度then heated
2. 2
   温度at reflux for 9 hours
3. 3
   workup.STIRRINGthe mixture was stirred
4. 4
   温度heated
5. 5
   温度at reflux for 1 hour
6. 6
   抽出the mixture was extracted with dichloromethane
7. 7
   乾燥dried (MgSO4)
8. 8
   ろ過filtered
9. 9
   その他The flitrate was evaporated to dryness
10. 10
    その他the residue was recrystallized from n-hexane

実験手順

A mixture of 2-nitro-4-trifluoromethylbenzonitrile (8.64 g), thiophenol (4.4 g) and potassium carbonate (6.9 g) in acetonitrile was stirred at room temperature for 1 hour then heated at reflux for 9 hours. Thiophenol (0.3 ml) was added and the mixture was stirred and heated at reflux for 1 hour. Water was added and the mixture was extracted with dichloromethane, dried (MgSO4) and filtered. The flitrate was evaporated to dryness and the residue was recrystallized from n-hexane to give 2-(phenylsulphenyl)-4-trifluoromethylbenzonitrile (9.5 g) as a white solid, m.p. 51° C.

出典