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Water → Ethyl 4-(2,5-dichlorobenzyl)piperazine-1-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1-Piperazinecarboxylic acid, ethyl ester | HCID 8431 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,5-Dichlorobenzyl chloride | HCID 75976 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Ethyl 4-(2,5-dichlorobenzyl)piperazine-1-carboxylate | HCID 22458123 | 63% |
反応手順
To a mixture comprising 1.94 g 1-ethoxycarbonylpiperazine and 3.45 g anhydrous potassium carbonate, in 20 mL of N,N-dimethylformamide, stirred at room temperature, under a nitrogen atmosphere, there was added 2.01 g of 2,5-dichlorobenzyl chloride. Then after 24 hr stirring at room temperature, this reaction mixture was poured into 200 mL of water, followed by extraction with ethyl acetate (3×100 mL). The obtained organic phase was dried over anhydrous sodium sulphate, followed by evaporation under vacuum. The obtained residue was then purified by flash chromatography (petroleum ether—ethyl acetate 85:15). The solvents were then evaporated off completely to give 2 g of Compound 14A (yield 63%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06271234B1 |
| 出典データセット | uspto-grants-2001_08 |
| ORD ID | ord-d159fbbd55bd4a90934b9504fd409427 |
| 出典メモ | uspto-grants-2001_08 |