Hydrochloric Acid → Da-6886
反応式
[NH2:1][C:2]1[C:10]([Cl:11])=[CH:9][C:5](C(N)=O)=[C:4]([O:12][CH3:13])[C:3]=1CC1CCNCC1.Cl.CS(O[CH2:27][CH2:28][CH2:29][N:30]1[CH:34]=[CH:33][N:32]=[N:31]1)(=O)=O.C([N:37]([CH2:40][CH3:41])[CH2:38][CH3:39])C.[C:42](=O)([O-])[O-].[K+].[K+].[I-].[K+].[CH3:50][N:51](C)[CH:52]=[O:53]>>[N:30]1([CH2:29][CH2:28][CH2:27][N:37]2[CH2:38][CH2:39][CH:42]([CH2:50][NH:51][C:52](=[O:53])[C:5]3[CH:9]=[C:10]([Cl:11])[C:2]([NH2:1])=[CH:3][C:4]=3[O:12][CH3:13])[CH2:41][CH2:40]2)[CH:34]=[CH:33][N:32]=[N:31]1参加物
8
反応条件
- 温度
- 120 °C
実験手順
4-amino-5-chloro-2-methoxy-(piperidin-4-ylmethyl)benzamide (compound of formula 2) hydrochloride (400 mg, 1.2 mmol) was dissolved in dimethylformamide (10 mL), and 3-(1,2,3-triazol-1-yl)propyl methanesulfonate (compound of formula 3) (344 mg, 1.68 mmol), triethylamine (0.5 mL, 3.591 mmol), potassium carbonate (232 mg, 1.68 mmol), and potassium iodide (40 mg, 0.24 mmol) were added thereto, followed by stirring at 120° C. for 4 hours. After the reaction was completed, the reactants were cooled to room temperature, extracted with ethyl acetate and water, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The resulting residue was purified by column chromatography to afford the title compound (185 mg, 38%).
後処理
- temperaturethe reactants were cooled to room temperature
- extractionextracted with ethyl acetate and water
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe resulting residue was purified by column chromatography
出典と根拠
- ORDレコード
- ord-a4574c81ae6b45b2bf0de9ec33dfeb9c
- 出典データセット
- uspto-grants-2015_12
- 特許番号
- US09221790B2
反応ノート
読み込み中…