반응 #443812

반응 방정식

5-bromo-o-anisaldehyde

ethylene glycol

ethylene glycol

→

2-(5-bromo-2-methoxyphenyl)-1,3-dioxolane

수율 126.5%

용매

toluene

반응 조건

후처리

1. 1
   온도at reflux for 21 hr
2. 2
   온도heated
3. 3
   온도at reflux for 6 hr
4. 4
   세척The resulting solution was washed with sat. NaHCO3, water and brine
5. 5
   건조dried over MgSO4
6. 6
   농축concentrated in vacuo

실험 절차

A solution of 5-bromo-o-anisaldehyde (49.7 g, 231 mmol), ethylene glycol (17.2 g, 277 mmol) and p-toluene sulfonic acid (4.3 g, 23 mmol) in dry toluene (400 ml) was heated at reflux for 21 hr. And then ethylene glycol (4.3 g, 70 mmol) was added to the reaction mixture and heated at reflux for 6 hr. The resulting solution was washed with sat. NaHCO3, water and brine, dried over MgSO4 and concentrated in vacuo to give crude 2-(5-bromo-2-methoxyphenyl)-1,3-dioxolane (75.7 g) as a dark red oil. The residue was added NaHCO3 and then distilled to give 2-(5-bromo-2-methoxyphenyl)-1,3-dioxolane (52.8 g, 88.3%) as a colorless oil.

출처