반응 #77309

반응 방정식

1-(2-fluorophenyl)piperazine

2-iodoethanol

potassium carbonate

→

title compound

수율 65.9%

1-(2-Hydroxyethyl)-4-(2-fluorophenyl)piperazine

수율 65.9%

용매

dimethylformamide

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도at reflux for three hours
3. 3
   기타The solvent was removed in vacuo
4. 4
   기타the residue was purified by preparative thin-layer chomatography (silica gel, eluting with chloroform/methanol, 9:1)

실험 절차

A mixture of 1-(2-fluorophenyl)piperazine (0.50 g), 2-iodoethanol (0.48 g), and potassium carbonate (1.5 g) in dimethylformamide (7 mL) was heated at reflux for three hours. The solvent was removed in vacuo and the residue was purified by preparative thin-layer chomatography (silica gel, eluting with chloroform/methanol, 9:1), giving the title compound as a yellow oil (0.41 g, 65%). 1H NMR (300 MHz, CDCl3) δ7.09-6.90 (m, 4H), 3.67 (t, 2H, J=5.4 Hz), 3.13 (t, 4H, J=4.7 Hz), 2.76 (br s, 1H), 2.71 (t, 4H, J=4.8 Hz), 2.63 (t, 4H, J=5.4 Hz). 13C NMR (75 MHz, CDCl3) δ156.3 (d, J=244.1 Hz), 140.6 (d, J=8.8 Hz), 125.1 (d, J=3.4 Hz), 123.2 (d, J=8.1 Hz), 119.5 (d, J=2.9 Hz), 116.7 (d, J=20.6 Hz), 60.1, 58.4, 53.6 (2C), 51.2 (d, 2C, J=3.0 Hz).

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