Sodium Carbonate → 4-(2-Methoxyethyl)piperazine-1-carbaldehyde
反応式
[CH:1]([N:3]1[CH2:8][CH2:7][NH:6][CH2:5][CH2:4]1)=[O:2].C(=O)([O-])[O-].[Na+].[Na+].[CH3:15][O:16][CH2:17][CH2:18]Br>CO>[CH:1]([N:3]1[CH2:8][CH2:7][N:6]([CH2:18][CH2:17][O:16][CH3:15])[CH2:5][CH2:4]1)=[O:2]参加物
5
実験手順
To a solution of 37.1 g of N-formylpiperazine and 37.1 g of anhydrous sodium carbonate in 50 mL of methanol was added dropwise 53.15 g of methoxyethyl bromide, and the mixture was refluxed for 3.5 hours. After cooling to room temperature, insolubles were filtered out and the filtrate was concentrated. To the residue was added water and chloroform. After separating the organic layer, the aqueous layer was extracted with chloroform. The combined organic layer was dried over anhydrous magnesium sulfate and concentrated to give 57.2 g of the title compound.
後処理
- temperaturethe mixture was refluxed for 3.5 hours
- filtrationinsolubles were filtered out
- concentrationthe filtrate was concentrated
- additionTo the residue was added water and chloroform
- customAfter separating the organic layer
- extractionthe aqueous layer was extracted with chloroform
- dry with materialThe combined organic layer was dried over anhydrous magnesium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-aaaf1bfb69a940fe969a8ee59137fee5
- 出典データセット
- uspto-grants-1999_10
- 特許番号
- US05969138
反応ノート
読み込み中…