反応式
[S:1]1[C:5]([C:6]([OH:8])=[O:7])=[CH:4][CH:3]=[C:2]1[C:9]([OH:11])=[O:10].[C:12](=O)([O-])[O-].[Na+].[Na+].CI>CN(C=O)C>[CH3:12][O:7][C:6]([C:5]1[S:1][C:2]([C:9]([OH:11])=[O:10])=[CH:3][CH:4]=1)=[O:8]参加物
5
実験手順
1.72 g (10 mmol) of thiophene-2,5-dicarboxylic acid and 3.18 g (30 mmol) of sodium carbonate suspended in 25 mL of DMF were stirred with 623 μL of methyl iodide at room temperature overnight. The sodium salt of the desired product was extracted with water, and 12M of hydrochloric acid was added to the combined aqueous layer. The desired product was extracted with ethyl acetate, and the combined organic layer was washed with saturated aqueous ammonium chloride and dried over anhydrous magnesium sulfate. The desired product was purified by silica gel column chromatography to give 0.49 g of a colorless solid (yield 28%).
後処理
- extractionThe sodium salt of the desired product was extracted with water, and 12M of hydrochloric acid
- additionwas added to the combined aqueous layer
- extractionThe desired product was extracted with ethyl acetate
- washthe combined organic layer was washed with saturated aqueous ammonium chloride
- dry with materialdried over anhydrous magnesium sulfate
- customThe desired product was purified by silica gel column chromatography
出典と根拠
- ORDレコード
- ord-20ff9d668ba74d5ba34d3fbdb9664090
- 出典データセット
- uspto-grants-2011_11
- 特許番号
- US08053453B2
関連ノート
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