反应详情

温度

100 °C

5 ml of 1N hydrochloric acid are added to a solution of 0.47 g of 2-methylpropan-2-yl 4-[4-(6-cyanopyridin-3-yl)-9H-carbazol-9-yl]-2-(tetrahydro-2H-pyran-4-ylamino)benzoate in 4 ml of dioxane. The reaction mixture is heated at 100° C. in a microwave for 2 hours and then concentrated under reduced pressure. The residue is purified twice by silica gel chromatography, elution being carried out successively with a mixture of dichloromethane and methanol (98/2 by volume) and then with a mixture of cyclohexane and ethyl acetate (50/50 by volume), so as to give 150 mg of 4-[4-(6-cyanopyridin-3-yl)-9H-carbazol-9-yl]-2-(tetrahydro-2H-pyran-4-ylamino)benzoic acid in the form of a yellow powder, the characteristics of which are the following:

1. concentrationconcentrated under reduced pressure
2. customThe residue is purified twice by silica gel chromatography, elution
3. additionbeing carried out successively with a mixture of dichloromethane and methanol (98/2 by volume)
4. additionwith a mixture of cyclohexane and ethyl acetate (50/50 by volume)