反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]([CH:32]([CH3:34])[CH3:33])([C:30]#[N:31])[CH2:12][CH2:13][CH2:14][CH:15]2[CH2:24][C:23]3[C:18](=[CH:19][C:20]([O:27][CH3:28])=[C:21]([O:25][CH3:26])[CH:22]=3)[CH2:17][N:16]2[CH3:29])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[ClH:35].CCOCC>C(O)(C)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]([CH:32]([CH3:34])[CH3:33])([C:30]#[N:31])[CH2:12][CH2:13][CH2:14][CH:15]2[CH2:24][C:23]3[C:18](=[CH:19][C:20]([O:27][CH3:28])=[C:21]([O:25][CH3:26])[CH:22]=3)[CH2:17][N:16]2[CH3:29])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[ClH:35]参加物
5
実験手順
The free base, 3-[4-(3,4-dimethoxyphenyl)-4-isopropyl-4-cyanobutyl]-6,7-dimethoxy-N-methyl-1,2,3,4-tetrahydroisoquinoline (1, 15 g, 0.032 mol) was dissolved in isopropanol (70 mL) at 70° C., and 6M HCl in isopropanol (5.6 mL) slowly added. After cooling to room temperature, ether (40 mL) was added until the solution became cloudy (saturated), and the resulting mixture stirred overnight. The resulting solid was collected, washed thoroughly with ether-isopropanol (1:1, 50 mL), and dried in vacuo at 50° C. to yield 3-[4-(3,4-dimethoxyphenyl)-4-isopropyl-4-cyanobutyl]-6,7-dimethoxy-N-methyl-1,2,3,4-tetrahydroisoquinoline·HCl (1·HCl, 13.7 g, m.p. 115°-120° C.) as a white powder.
後処理
- customThe resulting solid was collected
- washwashed thoroughly with ether-isopropanol (1:1, 50 mL)
- customdried in vacuo at 50° C.
出典と根拠
- ORDレコード
- ord-f7b0d798c79c4e5d88ee89341c0c7a36
- 出典データセット
- uspto-grants-1986_09
- 特許番号
- US04613606
関連ノート
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