반응 #1253195

반응 방정식

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

N,N-Diisopropylethylamine

3,4-difluoronitrobenzene

→

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

용매

acetonitrile

반응 조건

후처리

1. 1
   온도the mixture heated
2. 2
   온도to reflux for 18 hours
3. 3
   기타The solvent is removed
4. 4
   기타the residue chromatographed (silica
5. 5
   세척eluting with a gradient
6. 6
   온도increasing in polarity from 0 to 4% methanol in dichloromethane)

실험 절차

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.

출처