반응 #73984

ord-b972cb7c15c5458b950f4d2b4e5536a5

반응 방정식

C=C(C)C(=O)Cl
methacryloyl chloride
C[Si](C)(C)CC#CO
trimethylsilyl propyn-1-ol
CCN(CC)CC
Et3N
C=C(C)C(=O)OCC#C[Si](C)(C)C
2-Methyl-acrylic acid 3-trimethylsilanyl-prop-2-ynyl ester

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

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

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08541448B2uspto-grants-2013_09