Reacción #78910

Ecuación de reacción

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

Disolventes

ethanol

brine

Condiciones de reacción

Tratamiento posterior

1. 1
   OtroThe resulting reaction mixture
2. 2
   Temperaturawas refluxed
3. 3
   Extracciónextracted with EtOAc until the aqueous layer
4. 4
   SecadoThe combined organics were dried over MgSO4
5. 5
   Concentraciónconcentrated on rotary evaporator
6. 6
   OtroThe desired product was purified by silica gel flash chromatography

Procedimiento

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.

Fuente