Bis(2-Methoxyethyl)amine → Bis-(2-methoxy-ethyl)-prop-2-ynyl-amine
反応式
[CH2:1](Br)[C:2]#[CH:3].[CH3:5][O:6][CH2:7][CH2:8][NH:9][CH2:10][CH2:11][O:12][CH3:13].C(=O)([O-])[O-].[Cs+].[Cs+]>CC(C)=O>[CH3:5][O:6][CH2:7][CH2:8][N:9]([CH2:10][CH2:11][O:12][CH3:13])[CH2:1][C:2]#[CH:3]参加物
5
実験手順
Propargyl bromide (17.8 g, 150 mmol) was added dropwise to a mixture of bis(2-methoxy-ethyl)amine (20 g, 150 mmol) and cesium carbonate (49 g, 150 mmol) in 350 mL of acetone. The mixture was stirred overnight under nitrogen at room temperature. The inorganic salts were then filtered off, and the solvent was removed. The residue was dissolved in saturated sodium bicarbonate solution and extracted with ethyl acetate. The organic extracts were then evaporated to give 20 g of bis-(2-methoxy-ethyl)-prop-2-ynyl-amine: mass spectrum (m/e): M+H 172.
後処理
- filtrationThe inorganic salts were then filtered off
- customthe solvent was removed
- dissolutionThe residue was dissolved in saturated sodium bicarbonate solution
- extractionextracted with ethyl acetate
- customThe organic extracts were then evaporated
出典と根拠
- ORDレコード
- ord-e6ac1cd2b602457aa42c512bbece87cf
- 出典データセット
- uspto-grants-2001_10
- 特許番号
- US06297258B1
反応ノート
読み込み中…