반응 #318501

반응 방정식

trimethylchlorosilane

3-bromo-4-fluoro-benzaldehyde

ethane-1,2-diol

→

3-bromo-4-fluoro-benzaldehyde ethyleneacetal

수율 85.0%

용매

toluene

반응 조건

후처리

1. 1
   온도After cooling to room temperature
2. 2
   건조The organic phase was dried over sodium sulphate
3. 3
   기타evaporated in vacuo
4. 4
   workup.DISTILLATIONThe residue was distilled in vacuo

실험 절차

26 g (0.24 mol) of trimethylchlorosilane were added to a mixture of 20.3 g (0.1 mol) of 3-bromo-4-fluoro-benzaldehyde and 6.8 g (0.11 mol) of ethane-1,2-diol and the mixture was heated to 100° C. for 3 hours. After cooling to room temperature, 100 ml of toluene were added and the mixture was shaken twice with 50 ml of ice-water each time. The organic phase was dried over sodium sulphate and evaporated in vacuo. The residue was distilled in vacuo. 21 g (85% of theory) of 3-bromo-4-fluoro-benzaldehyde ethyleneacetal were thus obtained in the form of a colorless oil with a boiling point of 79°-81° C./0.1 mm Hg.

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