反応式
Cl[C:2]1[S:3][C:4]([CH:7]=[O:8])=[CH:5][N:6]=1.C(=O)([O-])[O-].[K+].[K+].[NH:15]1[CH2:20][CH2:19][O:18][CH2:17][CH2:16]1.O>C(#N)C.C(OCC)(=O)C>[O:18]1[CH2:19][CH2:20][N:15]([C:2]2[S:3][C:4]([CH:7]=[O:8])=[CH:5][N:6]=2)[CH2:16][CH2:17]1参加物
7
実験手順
2-Chlorothiazole-5-carbaldehyde (200 mg, 1.36 mmol) was dissolved in acetonitrile (4 mL). To this, potassium carbonate (376 mg, 2.72 mmol) and morpholine (0.237 mL, 2.72 mmol) were added at room temperature and the mixture was stirred at the same temperature for 23.5 hours. After water was added to the reaction mixture, extraction with ethyl acetate was performed, followed by washing with brine and drying over anhydrous sodium sulfate. The solvent was evaporated off under reduced pressure, and the residue was purified by preparative thin-layer chromatography (chloroform/methanol=15/1) to give 2-morpholinothiazole-5-carbaldehyde (179 mg, yield: 66%).
後処理
- washby washing with brine
- dry with materialdrying over anhydrous sodium sulfate
- customThe solvent was evaporated off under reduced pressure
- customthe residue was purified by preparative thin-layer chromatography (chloroform/methanol=15/1)
出典と根拠
- ORDレコード
- ord-b45d16598c424fb1b190567e53e95327
- 出典データセット
- uspto-grants-2014_03
- 特許番号
- US08673908B2
関連ノート
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