Reacción #347899

Ecuación de reacción

5-methyl-1,4-benzodioxane

bromine

sodium hydrogen sulfite

→

6-bromo-5-methyl-1,4-benzodioxane

Rendimiento 98.3%

Disolventes

acetic acid

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.ADDITIONwas added dropwise to the solution
2. 2
   Extracciónextracted with diethyl ether
3. 3
   LavadoThe resulting diethyl ether layer was washed successively with a sodium hydrogen carbonate aqueous solution, water and saturated saline solution
4. 4
   Secadodried over anhydrous magnesium sulfate
5. 5
   Otrothe solvent was removed under reduced pressure

Procedimiento

In 30 ml of acetic acid, was dissolved 10 g of 5-methyl-1,4-benzodioxane and 11.8 g of bromine was added dropwise to the solution. After stirring for 30 minutes, the reaction mixture was poured into a sodium hydrogen sulfite aqueous solution and extracted with diethyl ether. The resulting diethyl ether layer was washed successively with a sodium hydrogen carbonate aqueous solution, water and saturated saline solution, dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure to obtain 15.0 g of 6-bromo-5-methyl-1,4-benzodioxane (bp. 126°-135° C. (7 mmHg)).

Fuente