Hydrogen Bromide → 4,4-Dimethyl-1,2,3,4-tetrahydroisoquinolin-6-ol
反応式
[CH3:1][C:2]1([CH3:14])[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([O:12]C)[CH:10]=2)[CH2:5][NH:4][CH2:3]1.Br>>[CH3:1][C:2]1([CH3:14])[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([OH:12])[CH:10]=2)[CH2:5][NH:4][CH2:3]1参加物
3
実験手順
A mixture of 4,4-dimethyl-6-methoxy-1,2,3,4-tetrahydroisoquinoline (23.9 g, 0.125 mol) and 48% aqueous hydrobromic acid (158 ml) were heated at vigorous reflux for 4 hours. The reaction mixture was cooled and evaporated in vacuo. The residue was triturated with diethyl ether (20 ml), 1:1 diethyl ether:thf (20 ml) and diethyl ether (3×20 ml) and dried in vacuo to afford the title compound as the hydrobromide salt (17.5 g, 53%).
後処理
- temperaturewere heated
- temperatureat vigorous reflux for 4 hours
- temperatureThe reaction mixture was cooled
- customevaporated in vacuo
- customThe residue was triturated with diethyl ether (20 ml), 1:1 diethyl ether
- dry with materialthf (20 ml) and diethyl ether (3×20 ml) and dried in vacuo
出典と根拠
- ORDレコード
- ord-345688938f544416823b06572b186a49
- 出典データセット
- uspto-grants-2002_03
- 特許番号
- US06358974B1
反応ノート
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