反応 #1253195

反応方程式

1-(2-Fluoroethyl)-2-oxopiperazine trifluoroacetate

N,N-Diisopropylethylamine

3,4-difluoronitrobenzene

→

3-fluoro-4-(4-{2-fluoroethyl}-3-oxopiperazin-1-yl)nitrobenzene

溶媒

acetonitrile

反応条件

後処理

1. 1
   温度the mixture heated
2. 2
   温度to reflux for 18 hours
3. 3
   その他The solvent is removed
4. 4
   その他the residue chromatographed (silica
5. 5
   洗浄eluting with a gradient
6. 6
   温度increasing in polarity from 0 to 4% methanol in dichloromethane)

実験手順

1-(2-Fluoroethyl)-2-oxopiperazine trifluoroacetate (6.1 g) is dissolved in acetonitrile (100 ml). N,N-Diisopropylethylamine (13 ml) is added to the mixture, followed by 3,4-difluoronitrobenzene (3.39 g) and the mixture heated to reflux for 18 hours. The solvent is removed and the residue chromatographed (silica; eluting with a gradient increasing in polarity from 0 to 4% methanol in dichloromethane) to give 3-fluoro-4-(4-{2-fluoroethyl}-3-oxopiperazin-1-yl)nitrobenzene.

出典