Hydrochloric Acid → 4-(2-Methyl-4-nitrophenoxy)piperidine--hydrogen chloride (1/1)
反応式
C([N:4]1[CH2:9][CH2:8][CH:7]([O:10][C:11]2[CH:16]=[CH:15][C:14]([N+:17]([O-:19])=[O:18])=[CH:13][C:12]=2[CH3:20])[CH2:6][CH2:5]1)(=O)C.[ClH:21].C(O)C>O>[ClH:21].[N+:17]([C:14]1[CH:15]=[CH:16][C:11]([O:10][CH:7]2[CH2:8][CH2:9][NH:4][CH2:5][CH2:6]2)=[C:12]([CH3:20])[CH:13]=1)([O-:19])=[O:18]参加物
5
実験手順
To 1-acetyl-4-(4-nitro-2-methylphenyloxy)piperidine (11.8 g) were added conc. hydrochloric acid (15 ml), ethanol (15 ml) and water (15 ml) and the mixture was heated under reflux overnight. The reaction mixture was concentrated under reduced pressure, the residue thus obtained was washed with ethyl ether and crystals were filtered off to obtain 4-(4-nitro-2-methylphenyloxy)piperidine hydrochloride (8.3 g) as white crystals, m.p. 204°-226° C.
後処理
- temperaturethe mixture was heated
- temperatureunder reflux overnight
- concentrationThe reaction mixture was concentrated under reduced pressure
- customthe residue thus obtained
- washwas washed with ethyl ether and crystals
- filtrationwere filtered off
出典と根拠
- ORDレコード
- ord-0749b75cb7a3407a8d78e2f757b2fc54
- 出典データセット
- uspto-grants-1996_12
- 特許番号
- US05580883
反応ノート
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