تفاعل #78910

معادلة التفاعل

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

المذيبات

ethanol

brine

ظروف التفاعل

المعالجة

1. 1
   أخرىThe resulting reaction mixture
2. 2
   درجة الحرارةwas refluxed
3. 3
   استخلاصextracted with EtOAc until the aqueous layer
4. 4
   تجفيفThe combined organics were dried over MgSO4
5. 5
   تركيزconcentrated on rotary evaporator
6. 6
   أخرىThe desired product was purified by silica gel flash chromatography

الإجراء التجريبي

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.

المصدر