Reaktion #78910

Reaktionsgleichung

4-Piperazin-1-ylmethyl-benzoic acid

4-Piperazin-1-ylmethyl-benzoic Acid

chloromethyl-phosphonic acid diethyl ester

potassium carbonate

→

4-[4-(diethoxy-phosphorylmethyl)-piperazin-1-ylmethyl]-benzoic Acid

Lösungsmittel

ethanol

brine

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe resulting reaction mixture
2. 2
   Temperaturwas refluxed
3. 3
   Extraktionextracted with EtOAc until the aqueous layer
4. 4
   TrocknenThe combined organics were dried over MgSO4
5. 5
   Einengenconcentrated on rotary evaporator
6. 6
   SonstigeThe desired product was purified by silica gel flash chromatography

Vorschrift

To a solution of 4-Piperazin-1-ylmethyl-benzoic acid (4c) and chloromethyl-phosphonic acid diethyl ester (4d) in ethanol was added potassium carbonate. The resulting reaction mixture was refluxed, then cooled to room temperature, diluted with brine, acidified to pH˜4, and extracted with EtOAc until the aqueous layer showed little or no evidence of product by HPLC. The combined organics were dried over MgSO4 and concentrated on rotary evaporator. The desired product was purified by silica gel flash chromatography.

Quelle