反応 #77214

反応方程式

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

溶媒

ethanol

brine

反応条件

後処理

1. 1
   その他The resulting reaction mixture
2. 2
   温度was refluxed
3. 3
   抽出extracted with EtOAc until the aqueous layer
4. 4
   乾燥The combined organics were dried over MgSO4
5. 5
   濃縮concentrated on rotary evaporator
6. 6
   その他The desired product was purified by silica gel flash chromatography

実験手順

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.

出典