Reaktion #77215

Reaktionsgleichung

4-Piperazin-1-ylmethyl-benzoic acid

4-Piperazin-1-ylmethyl-benzoic Acid

chloro-(dimethyl-phosphinoyl)-methane

potassium carbonate

ethanol

→

4-[4-(dimethyl-phosphinoylmethyl)-piperazin-1-ylmethyl]-benzoic Acid

Lösungsmittel

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 chloro-(dimethyl-phosphinoyl)-methane (5a) 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