関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | N-Benzylaminodiacetic acid | HCID 77606 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Ammonium formate | HCID 2723923 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-Benzylpiperazine-2,6-dione | HCID 560967 | 87% |
反応手順
A suspension of 2,2′-(benzylazanediyl)diacetic acid (5.0 g, 22.4 mmol) and ammonium formate (4.2 g, 67.2 mmol) in N,N-dimethylformamide (75 mL) was stirred to reflux (160° C.) for 2 days. After cooling to room temperature, the reaction mixture was diluted by successive addition of ethyl acetate (150 mL) and a saturated solution of sodium hydrogen carbonate (150 mL). The aqueous layer was extracted with ethyl acetate (2×150 mL) and the combined organic phases were washed with a saturated solution of sodium chloride (3×100 mL), dried over sodium sulfate, filtered and concentrated under vacuum to give the title product as a yellow liquid (3.96 g, 87%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08623865B2 |
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| 出典データセット | uspto-grants-2014_01 |
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| ORD ID | ord-48116873b693424a91ee82b72059115e |
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| 出典メモ | uspto-grants-2014_01 |
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