反应 #366880

反应方程式

Dysprosium (III) trifluoromethanesulfonate

anisole

2-ethylbutanoic acid

water

→

para-methoxy-2-ethylbutyrophenone

收率 44.0%

溶剂

toluene

反应条件

后处理

1. 1
   温度the mixture was cooled
2. 2
   萃取extracted with 3×25 mL water
3. 3
   其他The organic layer was dried
4. 4
   过滤filtered
5. 5
   浓缩concentrated down in vacuo

实验过程

Dysprosium (III) trifluoromethanesulfonate (3.66 g as a wet solid), anisole (1.08 g) and 2-ethylbutanoic acid (1.16 g) were refluxed together in 125 mL toluene with azeotropic removal of the lower water layer (Dean-Stark apparatus). After 48 hours, the mixture was cooled and extracted with 3×25 mL water, then by 2×25 mL saturated sodium bicarbonate solution. The organic layer was dried using anhydrous sodium sulfate, filtered, then concentrated down in vacuo to give para-methoxy-2-ethylbutyrophenone (0.90 g, 44% yield) as an amber-colored oil, which was practically pure by 1H NMR analysis. Removal of water from the three water extracts recovered 3.54 g as a damp, off-white solid.

来源