反应 #73984

ord-b972cb7c15c5458b950f4d2b4e5536a5

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他Any precipitated ammonium salts can be removed by filtration, and volatile components
  2. 2
    其他can be removed under reduced pressure
  3. 3
    其他The crude product is then purified by flash chromatography

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08541448B2uspto-grants-2013_09