反応式
CO[CH:3](OC)[CH:4]([NH2:6])[CH3:5].[C:9](N1C=CN=C1)(N1C=CN=C1)=[S:10].C(N(CC)CC)C.[N:28]1([CH2:33][CH2:34][CH2:35][O:36][C:37]2[CH:42]=[CH:41][C:40]([C:43]3([CH2:49][NH2:50])[CH2:48][CH2:47][O:46][CH2:45][CH2:44]3)=[CH:39][CH:38]=2)[CH2:32][CH2:31][CH2:30][CH2:29]1.Cl>CN(C=O)C>[CH3:3][C:4]1[N:6]=[C:9]([SH:10])[N:50]([CH2:49][C:43]2([C:40]3[CH:41]=[CH:42][C:37]([O:36][CH2:35][CH2:34][CH2:33][N:28]4[CH2:32][CH2:31][CH2:30][CH2:29]4)=[CH:38][CH:39]=3)[CH2:44][CH2:45][O:46][CH2:47][CH2:48]2)[CH:5]=1参加物
反応物 5
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 50 °C
実験手順
2-Aminopropionaldehyde dimethyl acetal (0.2 g, 1.7 mmol), thiocarbonyldiimidazole (0.36 g, 2.0 mmol) and triethylamine (0.23 ml, 1.7 mmol) were stirred in DMF (2.0 ml) at ambient temperature for 30 minutes before heating to 50° C. for 18 hours. {4-[4-(3-pyrrolidin-1-ylpropoxy)phenyl]tetrahydropyran-4-yl}methylamine (540 mg, 1.7 mmol) was added and stirred at ambient temperature for 4 hours. 2M HCl (6 ml) was added, stirred at 70° C. for 18 hours, then c.HCl (1.0 ml) was added and the mixture stirred at 110° C. for 18 hours. The reaction mixture was cooled and partitioned between ethyl acetate (100 ml) and dilute aqueous sodium carbonate (50 ml). The organics were dried over Na2SO4 and concentrated in vacuo to give the title compound as a grey solid (600 mg, 84%). LRMS ESI+ m/z 416 [M+H]+.
後処理
- stirringstirred at 70° C. for 18 hours
- stirringthe mixture stirred at 110° C. for 18 hours
- temperatureThe reaction mixture was cooled
- custompartitioned between ethyl acetate (100 ml) and dilute aqueous sodium carbonate (50 ml)
- dry with materialThe organics were dried over Na2SO4
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-b796efc69428456c880e5d7cce14c0cf
- 出典データセット
- uspto-grants-2008_11
- 特許番号
- US07456164B2
関連ノート
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