反应详情

A solution of 50 g (0.26 mol) of 2,2-dimethyl-6-hydroxychroman-4-one (Example 1a) in 500 ml of DMF was added dropwise to a suspension of 9.0 g (0.3 mol) of 80 percent sodium hydride in 500 ml of DMF. The mixture was stirred at RT for 90 min, 49 g (0.265 mol) of iodobutane were added and the mixture was stirred at RT for a further 90 min. The reaction mixture was then concentrated under reduced pressure and the residue was admixed with water and extracted repeatedly with EA. The organic phases were washed with 5 M aqueous sodium hydroxide solution, stirred with activated carbon and magnesium sulfate, filtered and concentrated. This procedure gave 57.6 g of 6-butoxy-2,2-dimethylchroman-4-one.

1. stirringthe mixture was stirred at RT for a further 90 min
2. concentrationThe reaction mixture was then concentrated under reduced pressure
3. extractionextracted repeatedly with EA
4. washThe organic phases were washed with 5 M aqueous sodium hydroxide solution
5. stirringstirred with activated carbon and magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated