反応 #83348

反応方程式

4-Chloroquinoline

4-nitrothiophenol

potassium carbonate

→

4-(4-nitrophenylthio)quinoline

収率 54.0%

溶媒

ethanol

反応条件

後処理

1. 1
   濃縮The reaction mixture was then concentrated
2. 2
   workup.ADDITIONethyl acetate was added
3. 3
   洗浄the solution washed with water
4. 4
   乾燥dried over sodium sulfate
5. 5
   濃縮concentrated
6. 6
   その他The product was purified by HPLC over silica gel
7. 7
   洗浄eluted with 20-40% ethyl acetate/hexane

実験手順

4-Chloroquinoline (32.3 mmoles, 5.2 g),4-nitrothiophenol (32.3 moles, 5.0 g) and potassium carbonate (32.3 moles, 4.46 g) were stirred at room temperature in 500 ml of ethanol for 16 hr. The reaction mixture was then concentrated, ethyl acetate was added and the solution washed with water, dried over sodium sulfate and concentrated. The product was purified by HPLC over silica gel eluted with 20-40% ethyl acetate/hexane to yield 4-(4-nitrophenylthio)quinoline 4.9 g, 54%. Mass Spec (FD) 282. Calculated for C15H10N2O2S: C, 63.82 H, 3.57 N, 9.92. Found: C, 65.09; H, 3.81; N, 10.02.

出典