Water → N-methoxy-N-propargyl-p-chlorobenzamide
反応式
[H-].[Na+].[CH3:3][O:4][NH:5][C:6](=[O:14])[C:7]1[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][CH:8]=1.[CH2:15](Br)[C:16]#[CH:17].O>O1CCCC1>[CH3:3][O:4][N:5]([CH2:17][C:16]#[CH:15])[C:6](=[O:14])[C:7]1[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][CH:8]=1参加物
6
実験手順
0.22 g of sodium hydride (60% in oil) was suspended in 10 ml of tetrahydrofuran, and 1.0 g of N-methoxy-p-chlorobenzamide and 0.68 g of propargyl bromide were added thereto in this order while being cooled with ice. The mixture was heat-refluxed for 8 hours. After completion of the reaction, water was added to the reaction solution, and the mixture was extracted with ethyl acetate. The extract was dried, concentrated and purified by silica gel column chromatography to obtain 0.44 g of N-methoxy-N-propargyl-p-chlorobenzamide.
後処理
- temperaturein this order while being cooled with ice
- temperatureThe mixture was heat-refluxed for 8 hours
- additionwas added to the reaction solution
- extractionthe mixture was extracted with ethyl acetate
- customThe extract was dried
- concentrationconcentrated
- custompurified by silica gel column chromatography
出典と根拠
- ORDレコード
- ord-70e031461ff64ee8941f84d430c91d71
- 出典データセット
- uspto-grants-1998_03
- 特許番号
- US05733935
反応ノート
読み込み中…