Water → 6-(Methylthio)-3-pyridinecarboxaldehyde
反応式
Cl[C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][N:3]=1.[CH3:10][S-:11].[Na+].O>CN(C=O)C>[CH3:10][S:11][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][N:3]=1参加物
5
実験手順
In DMF (5.0 mL) was dissolved 6-chloronicotinaldehyde (300 mg, 2.12 mmol). Sodium thiomethoxide (178 mg, 2.54 mmol) was added and the mixture was stirred at room temperature for 2 hours. Water was added to the reaction mixture. Extraction with ethyl acetate, washing with saturated brine and drying over anhydrous sodium sulfate were performed. After filtration, the solvent in the filtrate was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=4/1) to give 6-(methylthio)nicotinaldehyde (239 mg, 74%).
後処理
- extractionExtraction with ethyl acetate
- washwashing with saturated brine
- dry with materialdrying over anhydrous sodium sulfate
- filtrationAfter filtration
- customthe solvent in the filtrate was evaporated under reduced pressure
- customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=4/1)
出典と根拠
- ORDレコード
- ord-bede641e31474cfdb4de9d5e028b3bb0
- 出典データセット
- uspto-grants-2015_10
- 特許番号
- US09150569B2
反応ノート
読み込み中…