反応式
Cl[C:2]1[N:7]=[CH:6][C:5]([CH2:8][NH:9][C:10]([C:12]2[N:16]3[CH:17]=[CH:18][CH:19]=[C:20]([O:21][CH2:22][CH:23]4[CH2:28][CH2:27][CH2:26][CH2:25][CH2:24]4)[C:15]3=[N:14][C:13]=2[CH3:29])=[O:11])=[CH:4][CH:3]=1.[NH:30]1[CH2:35][CH2:34][CH2:33][CH:32]([C:36]([O:38][CH2:39][CH3:40])=[O:37])[CH2:31]1.[Cl-].[NH4+].C(OCC)(=O)C>CN1CCCC1=O>[CH:23]1([CH2:22][O:21][C:20]2[C:15]3[N:16]([C:12]([C:10]([NH:9][CH2:8][C:5]4[CH:4]=[CH:3][C:2]([N:30]5[CH2:35][CH2:34][CH2:33][CH:32]([C:36]([O:38][CH2:39][CH3:40])=[O:37])[CH2:31]5)=[N:7][CH:6]=4)=[O:11])=[C:13]([CH3:29])[N:14]=3)[CH:17]=[CH:18][CH:19]=2)[CH2:28][CH2:27][CH2:26][CH2:25][CH2:24]1参加物
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
To a solution of 70 mg of N-[(6-chloropyridin-3-yl)methyl]-8-(cyclohexylmethoxy)-2-methylimidazolo[1,2-a]pyridine-3-carboxamide in 1 mL of N-methyl-2-pyrrolidone was added 0.12 mL of ethyl piperidine-3-carboxylate to carry out a reaction at 240° C. for 50 minutes under microwave irradiation. To the reaction mixture were added a saturated aqueous ammonium chloride solution and ethyl acetate to carry out a layer separation operation. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the obtained residue was purified by silica gel column chromatography to obtain 43 mg of ethyl 1-{5-[({[8-(cyclohexylmethoxy)-2-methylimidazolo[1,2-a]pyridin-3-yl]carbonyl}amino)methyl]pyridin-2-yl}piperidine-3-carboxylate.
後処理
- customa reaction at 240° C. for 50 minutes
- customunder microwave irradiation
- customa layer separation operation
- washThe organic layer was washed with saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- customThe solvent was evaporated under reduced pressure
- customthe obtained residue was purified by silica gel column chromatography
出典と根拠
- ORDレコード
- ord-ea84972a54ae4ade9e1c17560f042844
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09447090B2
関連ノート
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