Nitric Acid → 3-Nitroxypropylamine nitrate
反応式
[NH2:1][CH2:2][CH2:3][CH2:4][OH:5].[N+:6]([O-:9])([OH:8])=[O:7]>C(OC(=O)C)(=O)C>[N+:6]([O-:9])([OH:8])=[O:7].[N+:6]([O:5][CH2:4][CH2:3][CH2:2][NH2:1])([O-:8])=[O:7]参加物
4
実験手順
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)+.
後処理
- waitat room temperature for 10 minutes
- customThe solvent was evaporated under vacuum at 40° C
- stirringThe residue was stirred in diethyl ether (200 mL) until the product
- customprecipitated
- filtrationThe mixture was filtered
- customthe white crystalline solid was dried in vacuo
出典と根拠
- ORDレコード
- ord-fd95e3c9024b41f58c60e5039c57717d
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07087630B2
反応ノート
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