반응 #216074

반응 방정식

water

triiodophenol

sodium hydride

1,3-bis-(methanesulfonyloxy) butane

→

desired product

수율 54.0%

1,3-Bis-(2,4,6-Triiodophenoxy)-butane

수율 54.0%

용매

DMF

Ethyl acetate

DMF

반응 조건

후처리

1. 1
   온도The mixture was heated to 90° C. for 6 hours
2. 2
   온도after cooling
3. 3
   workup.WAITto stand overnight
4. 4
   기타The precipitated solid was collected
5. 5
   기타dried

실험 절차

A mixture of triiodophenol (5.78 g, 12.3 mmol) and sodium hydride (0.49 g, 60% dispersion, 12.3 mmol) in DMF (15 ml) was stirred at room temperature for 1 hour and then a solution of 1,3-bis-(methanesulfonyloxy) butane (1.37 g, 5.58 mmol) in DMF (5 ml) was added. The mixture was heated to 90° C. for 6 hours and then poured into water after cooling. Ethyl acetate was added and the mixture was allowed to stand overnight. The precipitated solid was collected and dried to give 3.0 g (54%) of the desired product, Mp 173°-175° C.

출처