반응 #61682

반응 방정식

2,6-dibromo-4-fluorophenol

potassium carbonate

methyl iodide

→

1,3-Dibromo-5-fluoro-2-methoxybenzene

수율 99.1%

용매

acetone

반응 조건

후처리

1. 1
   온도The mixture was heated
2. 2
   온도to reflux for 1.5 hours
3. 3
   여과filtered
4. 4
   세척washing the filter cake with dichloromethane (2×1.5 L)
5. 5
   농축The filtrate was concentrated in vacuo at 40° C
6. 6
   여과filtered
7. 7
   농축concentrated in vacuo at 40° C.

실험 절차

To a stirred solution of 2,6-dibromo-4-fluorophenol (214.5 g, 0.794 mol) in acetone (4.3 L), potassium carbonate (120.6 g, 0.874 mol) and methyl iodide (54.4 mL, 0.874 mol) were added at room temperature. The mixture was heated to reflux for 1.5 hours cooled to 25° C. and filtered, washing the filter cake with dichloromethane (2×1.5 L). The filtrate was concentrated in vacuo at 40° C. The crude product was slurred in dichloromethane (1 L) for 30 minutes at 25° C., filtered and concentrated in vacuo at 40° C. to give 1,3-Dibromo-5-fluoro-2-methoxybenzene as an off-white crystalline solid (223.3 g, 98.9%).

출처