Hydrochloric Acid → 3-(3-Methoxyphenyl)piperidine hydrochloride
反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH2:7]OC2C=CC=CC=2)[CH:2]=1.[ClH:15].[CH3:16][OH:17]>O=[Pt]=O>[ClH:15].[CH3:16][O:17][C:3]1[CH:2]=[C:7]([CH:3]2[CH2:4][CH2:5][CH2:6][NH:1][CH2:2]2)[CH:6]=[CH:5][CH:4]=1参加物
5
実験手順
To a solution of 3-(3-pyridinyl)methoxybenzene (22.0 g, 0.099 mol) in methanol (250 ml), PtO2 (2 g) and conc. HCl (30 ml) were added and the mixture was hydrogenated at 0.34 MPa in a Parr apparatus. After complete hydrogenation, the catalyst was filtered off. Most of the solvent was evaporated, the residue was made alkaline with 1 M NaOH and extracted with ether. The ether-phase was dried (Na2SO4) and the solvent evaporated giving 18 g of the amine product. The hydrochloride was made and then recrystallized from ethanol/ether yielding 20.9 g (93%), mp. 137°-138.5° C.
後処理
- filtrationAfter complete hydrogenation, the catalyst was filtered off
- customMost of the solvent was evaporated
- extractionextracted with ether
- dry with materialThe ether-phase was dried (Na2SO4)
- customthe solvent evaporated
出典と根拠
- ORDレコード
- ord-c28aaeb70cda4b7ea2e5bb158ba6fb9f
- 出典データセット
- uspto-grants-1984_01
- 特許番号
- US04426386
反応ノート
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