反应详情

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-l,4benzodioxane (bp. 126°-135° C. (7 mmHg)). 1H-NMR (CDC13) δ(ppm): 2.25 (3H, s), 4.23 (4H, s), 6.60 (1H, d, J=8.9Hz), 6.99 (1H, d, J=8.9Hz).

1. additionwas added dropwise to the solution
2. extractionextracted with diethyl ether
3. washThe resulting diethyl ether layer was washed successively with a sodium hydrogen carbonate aqueous solution, water and saturated saline solution
4. dry with materialdried over anhydrous magnesium sulfate
5. customthe solvent was removed under reduced pressure