反応 #1846

反応方程式

4-bromoanisole

Magnesium

iodine

THF

1,2-dibromoethane

→

Anisylmagnesium Bromide

反応条件

後処理

1. 1
   温度at reflux for 15 min
2. 2
   workup.STIRRINGstirring
3. 3
   その他After an exothermic reaction
4. 4
   workup.STIRRINGstirring
5. 5
   その他was accompanied by a rise in temperature to 35° C
6. 6
   温度The mixture was cooled to 20° C.
7. 7
   温度with cooling
8. 8
   workup.STIRRINGStirring
9. 9
   workup.ADDITIONafter the addition

実験手順

Magnesium (36 g, 1.5 mol), iodine (a few crystals) and THF (1 L) were heated under nitrogen, with stirring, at reflux for 15 min. The mixture was cooled to 20° C., stirring stopped, and 1,2-dibromoethane (2.5 ml) added. After an exothermic reaction was observed (a few min) stirring was restarted which was accompanied by a rise in temperature to 35° C. The mixture was cooled to 20° C. and 4-bromoanisole slowly added over 1 h at 14°-18° C. with cooling. Stirring was continued for 10 min after the addition was complete.

出典