Triethylamine → Propargyl methacrylate silyl protected

HRID 45706

반응식

HRID 45706 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

반응물 3

HCID 8471TriethylamineHCID 13528Methacryloyl chlorideHCID 11147726Trimethylsilyl propyn-1-ol

생성물 1

HCID 57624376Propargyl methacrylate silyl protected

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

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

  1. customAny precipitated ammonium salts can be removed by filtration, and volatile components
  2. customcan be removed under reduced pressure
  3. 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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