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Nitric Acid → 3-Nitroxypropylamine nitrate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | 3-Amino-1-propanol | HCID 9086 | — |
| 溶媒 | Acetic Anhydride | HCID 7918 | — |
| 生成物 | 3-Nitroxypropylamine nitrate | HCID 22014591 | 80% |
反応手順
A solution of 3-amino-1-propanol (6.17 g, 82.2 mmol) was added, dropwise, to an ice-cooled solution of fuming nitric acid (12 mL) in acetic anhydride (50 mL). The reaction was stirred in an ice-bath for 10 minutes and then at room temperature for 10 minutes. The solvent was evaporated under vacuum at 40° C. The residue was stirred in diethyl ether (200 mL) until the product precipitated. The mixture was filtered and the white crystalline solid was dried in vacuo to give the title compound (12.1 g, 80% yield). 1H NMR (DMSO-d6) δ 4.57 (br. t, 2 H), 2.8–3.0 (m, 2H), 1.96 (m, 2H). 13C NMR (DMSO-d6) δ 70.9, 36.1, 24.5. MS(API) m/z 121 (M−NO3)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07087630B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-fd95e3c9024b41f58c60e5039c57717d |
| 出典メモ | uspto-grants-2006_08 |