反応 #6702

反応方程式

water

4-Bromobenzaldehyde

p-toluenesulfonic acid monohydrate

ethylene glycol

→

2-(4-bromophenyl)-1,3-dioxolane

溶媒

ethyl acetate

benzene

反応条件

後処理

1. 1
   洗浄This solution was washed twice with aqueous bicarbonate
2. 2
   乾燥dried over magnesium sulfate
3. 3
   濃縮concentrated under reduced pressure
4. 4
   その他A colorless oil was recovered

実験手順

4-Bromobenzaldehyde (3 g, 0.0162 mol) in benzene (60 mL) was treated with p-toluenesulfonic acid monohydrate (0.15 g, 0.79 mmol) and ethylene glycol (5 mL, 0.0896 mol). The reaction was refluxed under nitrogen with azeotropic removal of water. After 3 hours, the reaction was cooled to room temperature and diluted with an equal volume of ethyl acetate. This solution was washed twice with aqueous bicarbonate, dried over magnesium sulfate and concentrated under reduced pressure. A colorless oil was recovered. Yield=2.83 g (92%). TLC (5% ethyl acetate in hexanes) showed clean product, Rf=0.17.

出典