反应方程式
Cl.[CH2:2]=[C:3]1[C:8](=[O:9])[CH:7]2[CH2:10][CH2:11][N:4]1[CH2:5][CH2:6]2.O.C([N:15]([CH2:18][CH3:19])[CH2:16][CH3:17])C>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC>[CH2:3]([N:4]([CH2:2][CH:3]1[C:8](=[O:9])[CH:7]2[CH2:10][CH2:11][N:4]1[CH2:5][CH2:6]2)[CH2:5][C:6]1[CH:17]=[CH:16][N:15]=[CH:18][CH:19]=1)[CH3:2]参与物
反应条件
- 温度
- 80 °C
实验过程
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.
后处理
- customThe completion of reaction
- customThe reaction mixture was quenched with ice-cold water (10 ml)
- extractionextracted with dichloromethane (2×50 ml), organic layers
- washwere washed with 10% NaHCO3 solution, brine
- dry with materialdried over sodium sulphate
- filtrationfiltered
- concentrationconcentrated
来源与证据
- ORD记录
- ord-e5a1120a58cc4d9687d2bd7ad3177757
- 来源数据集
- uspto-grants-2010_07
- 专利号
- US07759361B2
关联笔记
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