反应详情

温度

70 °C

To a solution of 2.65 g of 3-(1-acetyl-3,3-dimethyl-2,3-dihydro-1H-indol-6-yl)-1-[(2-chloropyridin-4-yl)methyl]-5,5-dimethylimidazolidine-2,4-dione obtained in stage h) below in 30 mL of dioxane are added 33 mL of aqueous 1N hydrochloric acid solution. The reaction mixture is heated at 70° C. for 17 hours and concentrated under reduced pressure. The residue is diluted with 30 mL of water and poured into saturated aqueous sodium hydrogen carbonate solution, and the precipitate formed is filtered off, washed with four times 10 mL of water and dried to give 2.3 g of 1-[(2-chloropyridin-4-yl)methyl]-3-(3,3-dimethyl-2,3-dihydro-1H-indol-6-yl)-5,5-dimethylimidazolidine-2,4-dione in the form of a beige-coloured solid, the characteristics of which are as follows:

1. concentrationconcentrated under reduced pressure
2. additionThe residue is diluted with 30 mL of water
3. additionpoured into saturated aqueous sodium hydrogen carbonate solution
4. customthe precipitate formed
5. filtrationis filtered off
6. washwashed with four times 10 mL of water
7. customdried