반응 #78767

반응 방정식

3-(1,1,2,2-tetrafluoroethoxy)benzaldehyde

N-(3-phenoxyphenyl)-3-amino-1,1,1-trifluoro-2-propanol

→

3-(3-phenoxyphenyl)-2-[3-(1,1,2,2-tetrafluoro-ethoxy)phenyl]-5-(trifluoromethyl)oxazolidine

수율 92.0%

용매

toluene

반응 조건

후처리

1. 1
   여과The reaction mixture was filtered
2. 2
   기타to remove the sieves
3. 3
   workup.ADDITIONthe filtrate was diluted with ethyl acetate
4. 4
   세척The organic layer was washed with brine
5. 5
   건조dried (MgSO4)
6. 6
   기타evaporated

실험 절차

A toluene solution (5 mL) of 3-(1,1,2,2-tetrafluoroethoxy)benzaldehyde (0.45 g, 2.0 mol) and N-(3-phenoxyphenyl)-3-amino-1,1,1-trifluoro-2-propanol (0.60 g, 2.0 mmol) was refluxed in the presence of molecular sieves and ZnI2 (˜5 mg) for 18 h under N2. The reaction mixture was filtered to remove the sieves, and the filtrate was diluted with ethyl acetate. The organic layer was washed with brine, dried (MgSO4) and evaporated to give 0.92 g (92%) of the desired 3-(3-phenoxyphenyl)-2-[3-(1,1,2,2-tetrafluoro-ethoxy)phenyl]-5-(trifluoromethyl)oxazolidine product as a colorless oil. The formation of the desired product was monitored by the disappearance of the aldehyde peak (δ˜10) in the 1H NMR spectrum. HRMS calcd. 502.1253 [M+H]+, found: 502.1220.

출처