Hydrochloric Acid → SiraMesine, Lu-28-179
反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[C:10]([CH2:17][CH2:18][CH2:19][CH2:20][N:21]3[CH2:26][CH2:25][C:24]4([C:34]5[C:29](=[CH:30][CH:31]=[CH:32][CH:33]=5)[CH2:28][O:27]4)[CH2:23][CH2:22]3)=[CH:9]2)=[CH:4][CH:3]=1.[ClH:35]>>[ClH:35].[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[C:10]([CH2:17][CH2:18][CH2:19][CH2:20][N:21]3[CH2:22][CH2:23][C:24]4([C:34]5[C:29](=[CH:30][CH:31]=[CH:32][CH:33]=5)[CH2:28][O:27]4)[CH2:25][CH2:26]3)=[CH:9]2)=[CH:4][CH:3]=1参加物
3
反応条件
- 温度
- 45 °C
実験手順
1′-[4-[1-(4-fluorophenyl)-1H-indole-3-yl]-1-butyl]-spiro[isobenzofuran-1(3H),4′-piperidine] (10.3 g) and 2-propanole (100 ml) were heated to reflux. The solution was allowed to cool to 45° C. Aqueous hydrochloric acid (2.2 ml, 36%) was added dropwise and a precipitate of the title compound was formed. The suspension was heated to reflux and allowed to cool to ambient temperature. The suspension was cooled in ice, filtered off and dried. Yield: 10.1 g (90%). The salt is a mono salt and according to our investigations an anhydrate. KF: 0.51%; HPLC 100.8%; DSC (onset/peakmax) 222.5° C./223.8° C. CHN (calculated/measured): C: 73.38/73.13; H: 6.57/6.56; N: 5.70/5.80.
出典と根拠
- ORDレコード
- ord-9a150b695d7a4ff3a4c5d5d4c2763d0f
- 出典データセット
- uspto-grants-2005_01
- 特許番号
- US06844352B2
反応ノート
読み込み中…