تفاعل #457678

معادلة التفاعل

Monobromopentaerythritol

triethylorthoformate

ethanol

→

4-bromomethyl-2,6,7-Trioxabicyclo[2.2.2]Octane

ظروف التفاعل

المعالجة

1. 1
   أخرىequipped with a side arm
2. 2
   workup.DISTILLATIONto distill out
3. 3
   workup.ADDITIONThen about 100 ml dioctyl phthalate and a trace of anhydrous p-toluenesulfonic acid are added
4. 4
   درجة الحرارةUnder vacuum the mixture is heated to about 140°-150° C
5. 5
   أخرىPeriodically the collected crystals are removed from the cold finger

الإجراء التجريبي

Monobromopentaerythritol from A (10 g, 0.05 mole) and 9 ml triethylorthoformate (0.05 mole) are mixed in a sublimation apparatus equipped with a side arm. The mixture is heated to about 100° C. with magnetic stirring, and 1,5 equivalents of ethanol are allowed to distill out. Then about 100 ml dioctyl phthalate and a trace of anhydrous p-toluenesulfonic acid are added. Under vacuum the mixture is heated to about 140°-150° C. Periodically the collected crystals are removed from the cold finger. After about 3 hours no more compound sublimes. The yield of 4-bromoethyl-2,6,7-trioxabicyclo[2.2.2]octane is 6.5 g (60%).

المصدر