Dimethylformamide → 3-Methoxythiophene-2-carbaldehyde

HRID 1445327

反応式

HRID 1445327 の反応式
[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

  1. temperatureWhile cooling in ice
  2. additionthe reaction solution was added to ice
  3. extractionThe aqueous phase was extracted 3 times with 25 ml of diethyl ether each time
  4. washthe combined organic phases were then washed with 50 ml of saturated sodium chloride solution
  5. dry with materialdried over sodium sulfate
  6. 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

関連ノート

読み込み中…