参与物
| 角色 | 名称 | HCID | 投料 |
|---|
| 反应物 | 聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] | HCID 962 | — |
| 反应物 | 三乙胺 | HCID 8471 | — |
| 反应物 | 1-Azabicyclo(2.2.2)octan-3-one, 2-methylene-, hydrochloride (1:1) | HCID 18401284 | — |
| 催化剂 | 四丁基溴化铵 | HCID 74236 | — |
| 产物 | 2-[(Ethyl-pyridin-4-ylmethyl-amino)-methyl]-1-aza-bicyclo[2.2.2]octan-3-one | HCID 58899562 | — |
反应步骤
To a stirred solution of 2-methylene-3-quinuclidinone hydrochloride (0.5 g, 0.0036 mol) in water (3 ml) N-(4-pyridylmethyl)ethylamine (0.49 g, 0.0036 mol), triethylamine (1.09 g, 0.0108 mol) and tetra-n-butyl ammonium bromide (116 mg, 0.00036 mol) were added and the reaction mixture were allowed to stir at 80° C. for 18 h. The completion of reaction was monitored by tlc. The reaction mixture was quenched with ice-cold water (10 ml), extracted with dichloromethane (2×50 ml), organic layers were washed with 10% NaHCO3 solution, brine and dried over sodium sulphate, filtered and concentrated to get the crude product which was purified as yellow solids (200 mg, 22%) by flash column chromatography on neutral silica gel using chloroform as eluent.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 专利号 | US07759361B2 |
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| 来源数据集 | uspto-grants-2010_07 |
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| ORD ID | ord-e5a1120a58cc4d9687d2bd7ad3177757 |
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| 来源说明 | uspto-grants-2010_07 |
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