Triethylamine → Propargyl methacrylate silyl protected
反応式
[CH3:1][Si:2]([CH2:5][C:6]#[C:7][OH:8])([CH3:4])[CH3:3].CCN(CC)CC.[C:16](Cl)(=[O:20])[C:17]([CH3:19])=[CH2:18]>CCOCC>[CH3:1][Si:2]([CH3:4])([CH3:3])[C:5]#[C:6][CH2:7][O:8][C:16](=[O:20])[C:17]([CH3:19])=[CH2:18]参加物
5
実験手順
A solution of trimethylsilyl propyn-1-ol (1 g, 7.8 mmol) and Et3N (1.4 mL, 10 mmol) in Et2O (10 mL) is cooled to −20° C. and a solution of methacryloyl chloride (0.9 mL, 9.3 mmol) in Et2O (5 mL) is added dropwise over 1 h. The mixture is stirred at this temperature for 30 min, and then allowed to warm to ambient temperature overnight. Any precipitated ammonium salts can be removed by filtration, and volatile components can be removed under reduced pressure. The crude product is then purified by flash chromatography.
後処理
- customAny precipitated ammonium salts can be removed by filtration, and volatile components
- customcan be removed under reduced pressure
- customThe crude product is then purified by flash chromatography
出典と根拠
- ORDレコード
- ord-b972cb7c15c5458b950f4d2b4e5536a5
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08541448B2
反応ノート
読み込み中…