Hydrochloric Acid → Chf-1024
反応式
Br.[OH:2][C:3]1[C:12]([OH:13])=[CH:11][CH:10]=[C:9]2[C:4]=1[CH2:5][CH2:6][CH:7]([NH:15][CH3:16])[C:8]2=O.[ClH:17]>[Pd].O>[ClH:17].[OH:2][C:3]1[C:12]([OH:13])=[CH:11][CH:10]=[C:9]2[C:4]=1[CH2:5][CH2:6][CH:7]([NH:15][CH3:16])[CH2:8]2参加物
5
反応条件
- 温度
- 0 °C
実験手順
A mixture of 10.0 g of 5,6-dihydroxy-2-methylamino-1-tetralone hydrobromide, 2.0 g of Pd/C 5%, 90 ml of water and 10 ml of 37% HCl is hydrogenated in an autoclave (Hastelloy) (20 atm, 80° C.) for 8-9 hours, then is filtered washing with hot water. The aqueous solution is concentrated under vacuum and the resulting solid is warm triturated with 100 ml of 37% hydrochloric acid, then cooled to 0° C. and filtered. The resulting solid is recrystallized from acetone and dried under vacuum at 60° C. Yield: 7.4 g.
後処理
- filtrationis filtered
- washwashing with hot water
- concentrationThe aqueous solution is concentrated under vacuum
- temperaturethe resulting solid is warm
- customtriturated with 100 ml of 37% hydrochloric acid
- filtrationfiltered
- customThe resulting solid is recrystallized from acetone
- customdried under vacuum at 60° C
出典と根拠
- ORDレコード
- ord-3c7f8153ace74d128cd633f2b040357f
- 出典データセット
- uspto-grants-2000_03
- 特許番号
- US06034277
反応ノート
読み込み中…