Dimethylformamide → 3-Methoxythiophene-2-carbaldehyde
反応式
[CH3:1][O:2][C:3]1[CH:7]=[CH:6][S:5][CH:4]=1.P(Cl)(Cl)(Cl)=O.[OH-].[Na+].CN(C)[CH:17]=[O:18]>>[CH3:1][O:2][C:3]1[CH:7]=[CH:6][S:5][C:4]=1[CH:17]=[O:18]参加物
5
実験手順
1.03 ml of 3-methoxythiophene were dissolved in 2.3 ml of dimethylformamide. While cooling in ice, 1.06 ml of phosphoryl chloride were added. After 1 h, the reaction solution was added to ice, and the solution was neutralized with 5 molar sodium hydroxide solution. The aqueous phase was extracted 3 times with 25 ml of diethyl ether each time, and the combined organic phases were then washed with 50 ml of saturated sodium chloride solution, dried over sodium sulfate and concentrated. 840 mg of the product with the molecular mass of 142.18 (C6H7O2S) were obtained. MS (ESI): 143.0 (M+H+).
後処理
- temperatureWhile cooling in ice
- additionthe reaction solution was added to ice
- extractionThe aqueous phase was extracted 3 times with 25 ml of diethyl ether each time
- washthe combined organic phases were then washed with 50 ml of saturated sodium chloride solution
- dry with materialdried over sodium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-1210ce13762d499faf02c5899c975605
- 出典データセット
- uspto-grants-2010_02
- 特許番号
- US07666848B2
反応ノート
読み込み中…