Hydrochloric Acid → 6-[(Dimethylamino)methyl]-5,6,7,8-tetrahydronaphthalen-2-amine
反応式
Cl.C([NH:5][C:6]1[CH:7]=[C:8]2[C:13](=[CH:14][CH:15]=1)[CH2:12][CH:11]([CH2:16][N:17]([CH3:19])[CH3:18])[CH2:10][CH2:9]2)(=O)C.Cl.[OH-].[Na+]>>[NH2:5][C:6]1[CH:7]=[C:8]2[C:13](=[CH:14][CH:15]=1)[CH2:12][CH:11]([CH2:16][N:17]([CH3:19])[CH3:18])[CH2:10][CH2:9]2参加物
4
実験手順
6-Acetylamino-2-(N,N-dimethylamino)methyltetralin hydrochloride (0.879 g; obtained in Reference Example 31) was added to 2 N hydrochloric acid. The reaction mixture was heated under reflux for 90 minutes, and then an aqueous solution of 1 N sodium hydroxide was added thereto to thereby make the resulting mixture have pH of 9. Then, this was extracted with ethyl acetate. The organic layer was washed with water and a saturated aqueous sodium chloride solution, then dried, and concentrated. The residue was purified by alumina column chromatography (eluent: ethyl acetate/hexane=1/1) to obtain the entitled compound (0.231 g).
後処理
- temperatureThe reaction mixture was heated
- temperatureunder reflux for 90 minutes
- extractionThen, this was extracted with ethyl acetate
- washThe organic layer was washed with water
- dry with materiala saturated aqueous sodium chloride solution, then dried
- concentrationconcentrated
- customThe residue was purified by alumina column chromatography (eluent: ethyl acetate/hexane=1/1)
出典と根拠
- ORDレコード
- ord-146cfd21403046fda72e7ae17a8fbb01
- 出典データセット
- uspto-grants-2003_09
- 特許番号
- US06613805B2
反応ノート
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