반응 #1846

반응 방정식

4-bromoanisole

Magnesium

iodine

THF

1,2-dibromoethane

→

Anisylmagnesium Bromide

반응 조건

후처리

1. 1
   온도at reflux for 15 min
2. 2
   workup.STIRRINGstirring
3. 3
   기타After an exothermic reaction
4. 4
   workup.STIRRINGstirring
5. 5
   기타was accompanied by a rise in temperature to 35° C
6. 6
   온도The mixture was cooled to 20° C.
7. 7
   온도with cooling
8. 8
   workup.STIRRINGStirring
9. 9
   workup.ADDITIONafter the addition

실험 절차

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.

출처