Triethylamine → Propargyl methacrylate silyl protected
반응식
[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]참가 물질
5
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-b972cb7c15c5458b950f4d2b4e5536a5
- 출처 데이터셋
- uspto-grants-2013_09
- 특허 번호
- US08541448B2
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