Hydrochloric Acid → 5-Nitro-indan-2-ylamine hydrochloride
반응식
[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]1참가 물질
3
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-c3760d2e17784bd7bf76d4a442173bbc
- 출처 데이터셋
- uspto-grants-2001_03
- 특허 번호
- US06197798B1
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