Water → Prop-2-yn-1-yl benzoate
反応式
[CH2:1](O)[C:2]#[CH:3].C(Cl)Cl.CCN(CC)CC.[C:15](Cl)(=[O:22])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.[OH2:24]>CN(C1C=CN=CC=1)C>[C:15]([O:22][CH2:3][C:2]#[CH:1])(=[O:24])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1参加物
7
実験手順
To a solution of prop-2-yn-1-ol (3.63 mL, 62.4 mmol), DCM (180 mL), and Et3N (17.40 mL, 125 mmol) at 0° C. were added benzoyl chloride (7.25 mL, 62.4 mmol) and DMAP (0.381 g, 3.12 mmol). The reaction was stirred while warming to room temperature overnight. The reaction was diluted with water and the layers separated. The aqueous was extracted with DCM and the combined organics were dried over Na2SO4, filtered, and concentrated to afford prop-2-yn-1-yl benzoate which was used in subsequent reactions without further purification. LC/MS m/z 161 [M+H]+.
後処理
- customthe layers separated
- extractionThe aqueous was extracted with DCM
- dry with materialthe combined organics were dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-d977b2d89431403f8dfe35413140fc84
- 出典データセット
- uspto-grants-2014_08
- 特許番号
- US08796261B2
反応ノート
読み込み中…