Reaktion #1379289

Reaktionsgleichung

1-[4-(4-fluorobenzyloxy)-3-isobutylbenzoyl]-4-(2-hydroxyethyl) piperazine

piperonyloyl chloride

→

aimed compound

Ausbeute 72.5%

1-[4-(4-fluorobenzyloxy)-3-isobutylbenzoyl]-4-[2-(piperonyloyloxy)ethyl]piperazine

Ausbeute 72.5%

Lösungsmittel

dichloromethane

triethylamine

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas added
2. 2
   Waschenthe reaction mixture was washed with saturated aqueous sodium hydrogencarbonate solution and saturated brine successively
3. 3
   Trocknendried over sodium sulfate anhydride
4. 4
   Einengenconcentrated under a vacuum
5. 5
   SonstigeThus obtained residue was purified by silica gel column chromatography (chloroform:methanol=50:1)

Vorschrift

1-[4-(4-fluorobenzyloxy)-3-isobutylbenzoyl]-4-(2-hydroxyethyl) piperazine (1.95 g) was dissolved in a mixture of dichloromethane (30 ml) and triethylamine (1.04 ml) and then, while being cooled with ice, piperonyloyl chloride (0.93 g) was added thereto dropwise. After being stirred for 12 hours at room temperature, the reaction mixture was washed with saturated aqueous sodium hydrogencarbonate solution and saturated brine successively, dried over sodium sulfate anhydride, and then concentrated under a vacuum. Thus obtained residue was purified by silica gel column chromatography (chloroform:methanol=50:1), thereby yielding 1.92 g of the aimed compound.

Quelle