反应详情

To the solution of 4-hydroxymethyl-2,6-bis-pentyloxyphenol (525 mg, 1.62 mmol), 1-(4-fluorophenyl)-2-piperazine-1-yl-ethanone (432 mg, 1.94 mmol) and PPh3 (509 mg, 1.94 mmol) in drying THF (10 ml) was dropped diethyl azodicarboxylate (0.38 ml, 2.43 mmol) at 0° C. and then was stirred 15 minutes at room temperature. The solution was added with H2O, then CH2Cl2 was evaporated in vacuo and was washed with brine. The obtained organic solution was dried over anhydrous magnesium sulfate and filtered. The obtained filterate was vacuum concentrated to give the residue, which was purified by column chromatography (Hexane:EtOAc=1:10), yielding 129 mg (15%) of 1-(4-fluorophenyl)-2-[4-(4-hydroxy -3,5-bis-pentyloxybenzyl)piperizine-1-yl]ethanone as a yellow oil.

1. customCH2Cl2 was evaporated in vacuo
2. washwas washed with brine
3. dry with materialThe obtained organic solution was dried over anhydrous magnesium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. customto give the residue, which
7. customwas purified by column chromatography (Hexane:EtOAc=1:10)