反应详情

温度

90 °C

0.3 g of potassium carbonate and 1.68 g of 4-trans-aminocyclohexanol are successively added to a solution of 0.34 g of 2-methylpropan-2-yl 4-[4-(6-cyanopyridin-3-yl)-9H-carbazol-9-yl]-2-fluorobenzoate in 6 ml of dimethyl sulphoxide. The reaction mixture is heated at 90° C. for 2 hours in a microwave, 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 to dryness under reduced pressure. The residue is purified by silica gel chromatography, elution being carried out with a mixture of cyclohexane and ethyl acetate (75/25 by volume), so as to give 0.15 g of 2-methylpropan-2-yl 4-[4-(6-cyanopyridin-3-yl)-9H-carbazol-9-yl]-2-[(trans-4-hydroxycyclohexyl)amino]benzoate 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 to dryness under reduced pressure
5. customThe residue is purified by silica gel chromatography, elution
6. additionbeing carried out with a mixture of cyclohexane and ethyl acetate (75/25 by volume)