反应详情

温度

90 °C

0.17 g of potassium carbonate and 0.64 ml of 3-amino-1-propanol are successively added to a solution of 0.18 g of 2-fluoro-4-{4-[6-(trifluoromethyl)pyridin-3-yl]-9H-carbazol-9-yl}benzonitrile in 2 ml of dimethyl sulphoxide. The reaction mixture is heated at 90° C. for 1 hour 20 minutes in a microwave, and then 4.2 ml of ethanol are added, followed by 0.8 ml of a 1N solution of sodium hydroxide and 0.8 ml of 30% aqueous hydrogen peroxide. The reaction mixture is stirred at ambient temperature for 2 hours and then diluted with distilled water. The aqueous phase is extracted twice with ethyl acetate and the combined organic phases are washed with water and a saturated solution of sodium chloride, dried over magnesium sulphate and concentrated under reduced pressure. The white solid obtained is purified by silica gel chromatography, elution being carried out with a mixture of dichloromethane, acetonitrile and methanol (96/2/2 by volume) so as to give 24 mg of 2-[(3-hydroxypropyl)amino]-4-{4-[6-(trifluoromethyl)pyridin-3-yl]-9H-carbazol-9-yl}benzamide in the form of a white solid, the characteristics of which are the following

1. extractionThe aqueous phase is extracted twice with ethyl acetate
2. washthe combined organic phases are washed with water
3. dry with materiala saturated solution of sodium chloride, dried over magnesium sulphate
4. concentrationconcentrated under reduced pressure
5. customThe white solid obtained
6. customis purified by silica gel chromatography, elution
7. additionbeing carried out with a mixture of dichloromethane, acetonitrile and methanol (96/2/2 by volume) so as