関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrogen Bromide | HCID 260 | — |
| 反応物 | Ethyl 4-benzylhomopiperazine-1-carboxylate | HCID 54118699 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-Benzyl-1,4-diazepane | HCID 228365 | 89.2% |
反応手順
A mixture of 0.85 g of ethyl 4-benzylhomopiperazine-1-carboxylate and 5 ml of 47% hydrobromic acid was heated at 100° C. for 10 hours. After addition of a small amount of water, the reaction mixture was washed with ethyl acetate. The aqueous layer was made alkaline with 30% sodium hydroxide and, after salting out with sodium chloride, extracted with ethyl acetate. The organic layer was washed with saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate and concentrated under reduced pressure to give 0.55 g of 1-benzylhomopiperazine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04987132 |
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| 出典データセット | uspto-grants-1991_01 |
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| ORD ID | ord-2d4cbe5d0ee0429bb7fd06053c051ddc |
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| 出典メモ | uspto-grants-1991_01 |
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