Реакция #77214

Уравнение реакции

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

Растворители

ethanol

brine

Условия реакции

Обработка

1. 1
   ДругоеThe resulting reaction mixture
2. 2
   Температураwas refluxed
3. 3
   Экстракцияextracted with EtOAc until the aqueous layer
4. 4
   СушкаThe combined organics were dried over MgSO4
5. 5
   Концентрированиеconcentrated on rotary evaporator
6. 6
   ДругоеThe desired product was purified by silica gel flash chromatography

Методика

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.

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