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Potassium Carbonate → 4-[4-(Diethoxy-phosphorylmethyl)-piperazin-1-ylmethyl]-benzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Phosphonic acid, P-(chloromethyl)-, diethyl ester | HCID 76633 | — |
| 反応物 | 4-(1-Piperazinylmethyl)benzoic acid | HCID 17606055 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | 4-[4-(Diethoxy-phosphorylmethyl)-piperazin-1-ylmethyl]-benzoic acid | HCID 20634549 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06713462B2 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-67e25cb957584aa59a373f9e477579a2 |
| 出典メモ | uspto-grants-2004_03 |