反应详情

A solution of 50 g (0.26 mol) of 2,2-dimethyl-6-hydroxychroman-4-one (Example 28a) in 500 ml of DMF was added dropwise to a suspension of 9.0 g (0.3 mol) of 80% sodium hydride in 500 ml of DMF. After stirring 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 in vacuo, the residue was treated with water and the mixture was extracted several times with EA. The organic phases were washed with 5 M sodium hydroxide solution, stirred with activated carbon and magnesium sulfate, filtered and concentrated. 57.6 g of 6-butoxy-2,2-dimethylchroman-4-one were obtained.

1. stirringthe mixture was stirred at RT for a further 90 min
2. concentrationThe reaction mixture was then concentrated in vacuo
3. additionthe residue was treated with water
4. extractionthe mixture was extracted several times with EA
5. washThe organic phases were washed with 5 M sodium hydroxide solution
6. stirringstirred with activated carbon and magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated