Triethylamine → Propargyl methacrylate silyl protected

HRID 45706

反応式

HRID 45706 の反応式
[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

反応物 3

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

生成物 1

HCID 57624376Propargyl methacrylate silyl protected

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

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

  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

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

関連ノート

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