反応式
Cl[C:2]1[C:7]2[CH:8]=[C:9]([S:11]([O-:13])=[O:12])[S:10][C:6]=2[CH:5]=[CH:4][N:3]=1.[Li+].[Br:15][C:16]1[CH:17]=[C:18]([CH:21]=[CH:22][CH:23]=1)[CH2:19]Br.[C:24]([O:28][C:29]([N:31]1[CH2:36][CH2:35][NH:34][CH2:33][CH2:32]1)=[O:30])([CH3:27])([CH3:26])[CH3:25]>C(#N)C>[C:24]([O:28][C:29]([N:31]1[CH2:36][CH2:35][N:34]([C:2]2[C:7]3[CH:8]=[C:9]([S:11]([CH2:19][C:18]4[CH:21]=[CH:22][CH:23]=[C:16]([Br:15])[CH:17]=4)(=[O:13])=[O:12])[S:10][C:6]=3[CH:5]=[CH:4][N:3]=2)[CH2:33][CH2:32]1)=[O:30])([CH3:27])([CH3:25])[CH3:26]参加物
5
実験手順
Lithium 4-chlorothieno[3,2-c]pyridine-2-sulfinate (0.44 mmol) was treated with 3-bromobenzylbromide (0.59 mmol) as described in Method P above and then reacted further with tert-butyl-piperazine-1-carboxylate as described in Method Q. Yield 0.023 g (10% over two steps). Beige solid. 1H NMR (300 MHz, CDCl3) δ 8.16 (d, J=6 Hz, 1H), 7.50-7.55 (m, 2H), 7.32-7.40 (m, 2H), 7.10-7.24 (m, 3H), 4.44 (s, 2H), 3.61-3.73 (m, 8H), 1.50 (s, 9H); MS (ESI+) for C23H26BrN3O4S2 m/z 554 (M+H)+. HPLC 77%, RT 4.07 min (ACE3 C8 50×4.6 mm, 5-50% acetonitrile in 3 min).
出典と根拠
- ORDレコード
- ord-f2dc88b6f5a14f34a03f99993a57197e
- 出典データセット
- uspto-grants-2011_05
- 特許番号
- US07943639B2
関連ノート
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