Hydrogen Bromide → Desacetyl-7-desmethyl Agomelatine Hydrobromide
反応式
Cl.C[O:3][C:4]1[CH:13]=[C:12]2[C:7]([CH:8]=[CH:9][CH:10]=[C:11]2[CH2:14][CH2:15][NH2:16])=[CH:6][CH:5]=1.[BrH:17]>>[BrH:17].[OH:3][C:4]1[CH:13]=[C:12]2[C:7]([CH:8]=[CH:9][CH:10]=[C:11]2[CH2:14][CH2:15][NH2:16])=[CH:6][CH:5]=1参加物
3
実験手順
13.8 g (5.81×10-2 mol) of 2-(7-methoxy-1-naphthyl)ethylamine hydrochloride and 46 cm3 of 47% hydrobromic acid solution are introduced into a 250-cm3 round- bottom flask with a ground neck. The mixture is brought to reflux for 6.5 hours. After cooling, the reaction medium is filtered. The precipitate is washed with water and then with hexane. Recrystallization of the crude product is carried out in an ethyl acetate/hexane mixture to obtain 2-(7-hydroxy-1-naphthyl)ethylamine hydrobromide (yield 80%; melting point: 174°-175° C.).
後処理
- temperatureto reflux for 6.5 hours
- temperatureAfter cooling
- filtrationthe reaction medium is filtered
- washThe precipitate is washed with water
- customRecrystallization of the crude product
出典と根拠
- ORDレコード
- ord-fd5b207a0985418fae5caa7753715d24
- 出典データセット
- uspto-grants-1995_05
- 特許番号
- US05420158
反応ノート
読み込み中…