Hydrochloric Acid → 5-Nitro-indan-2-ylamine hydrochloride
反応式
[N+:1]([C:4]1[CH:5]=[C:6]2[C:10](=[CH:11][CH:12]=1)[CH2:9][CH:8]([NH:13]C(=O)C)[CH2:7]2)([O-:3])=[O:2].[ClH:17]>>[ClH:17].[NH2:13][CH:8]1[CH2:7][C:6]2[C:10](=[CH:11][CH:12]=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=2)[CH2:9]1参加物
3
実験手順
To N-(5-nitro-indan-2-yl)-acetamide (23.5 g, 107 mmol) is added 2N hydrochloric acid (500 mL). The mixture is heated to reflux for 24 h and then concentrated in vacuo. Methanol (100 mL) is added to the residue and the mixture is concentrated in vacuo. Toluene (100 mL) is added and the mixture is again concentrated. A solution of the residue in methanol (100 mL) is warmed, diethyl ether (500 mL) is added and the mixture is let stand overnight. The solid is collected by filtration and air dried to yield 2-amino-5-nitro-indane hydrochloride as a white solid.
後処理
- temperatureThe mixture is heated
- temperatureto reflux for 24 h
- concentrationconcentrated in vacuo
- additionMethanol (100 mL) is added to the residue
- concentrationthe mixture is concentrated in vacuo
- additionToluene (100 mL) is added
- concentrationthe mixture is again concentrated
- temperatureA solution of the residue in methanol (100 mL) is warmed
- additiondiethyl ether (500 mL) is added
- filtrationThe solid is collected by filtration and air
- customdried
出典と根拠
- ORDレコード
- ord-c3760d2e17784bd7bf76d4a442173bbc
- 出典データセット
- uspto-grants-2001_03
- 特許番号
- US06197798B1
反応ノート
読み込み中…