N-BOC-哌嗪 → HCID 67157767，化合物

HRID 549299

反应方程式

HRID 549299 反应方程式
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+].[CH3:15][O:16][C:17]1[CH:18]=[C:19]([CH:22]=[C:23]([O:25][CH3:26])[CH:24]=1)[CH2:20]Br.[C:27]([O:31][C:32]([N:34]1[CH2:39][CH2:38][NH:37][CH2:36][CH2:35]1)=[O:33])([CH3:30])([CH3:29])[CH3:28]>C(#N)C>[CH3:15][O:16][C:17]1[CH:18]=[C:19]([CH:22]=[C:23]([O:25][CH3:26])[CH:24]=1)[CH2:20][S:11]([C:9]1[S:10][C:6]2[CH:5]=[CH:4][N:3]=[C:2]([N:37]3[CH2:36][CH2:35][N:34]([C:32]([O:31][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:33])[CH2:39][CH2:38]3)[C:7]=2[CH:8]=1)(=[O:13])=[O:12]

参与物

5

反应物 3

HCID 143452N-BOC-哌嗪HCID 12744903,5-二甲氧基溴苄HCID 86591057HCID 86591057，化合物

产物 1

HCID 67157767HCID 67157767，化合物

试剂、催化剂与溶剂 1

HCID 6342乙腈溶剂

实验过程

Lithium 4-chlorothieno[3,2-c]pyridine-2-sulfinate (0.44 mmol) was treated with 3,5-dimethoxybenzylbromide (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 0.02 g (10% over two steps). Beige solid. 1H NMR (300 MHz, CDCl3) δ 8.14-8.18 (m, 1H), 7.55 (s, 1H), 6.40-6.45 (m, 1H), 6.26-6.34 (m, 2H), 4.39 (s, 2H), 3.54-3.72 (m, 14H), 1.50 (s, 9H); MS (ESI+) for C25H31N3O6S2 m/z 534 (M+H)+. HPLC 69%, RT 1.99 min (YMC ODS AQ, 33×3 mm, 10-90% acetonitrile in 3 min).

来源与证据

ORD记录
ord-2b71d6e9c29d40809b7654d59228011e
来源数据集
uspto-grants-2011_05
专利号
US07943639B2

关联笔记

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