达芦那韦

反应条件: temp:115.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Darunavir Ethanolate (5.0 g) was suspended into glycerol (25 g), heated to 110-120° C. under vacuum and maintained for 30 min. Water (50 mL) was added to the cooled reaction mass at 25-35° C. under stirring and the obtained suspension was stirred for 30 min at 25-35° C. The separated solid was filtered and dried at 40-45° C. under vacuum to yield 3.5 g of amorphous Darunavir. maintained for 30 min the obtained suspension was stirred for 30 min at 25-35° C The separated solid was filtered dried at 40-45° C. under vacuum

反应条件: temp:42.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Darunavir Ethanolate (10 g) was dissolved in ethyl acetate (50 mL). The solution was heated to 40-45° C. and maintained for 30 min. Ethyl acetate was distilled off under vacuum completely to get residue in the form of semisolid. n-Heptane (50 mL) was added to the residue and stirred for 30 min. at ambient temperature. The separated solid was filtered, washed the wet cake with n-heptane (5 mL) and dried at 40-45° C. under vacuum to get 8.0 g of amorphous Darunavir. maintained for 30 min Ethyl acetate was distilled off under vacuum completely to get residue in the form of semisolid The separated solid was filtered washed the wet cake with n-heptane (5 mL) dried at 40-45° C. under vacuum

反应条件: temp:72.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 100 gm of darunavir was dissolved in 1000 ml of denatured ethanol (mixture of 97% ethanol and 3% toluene) at 70-75° C. to obtain clear solution. 5 gm of activated charcoal was added and stirred for 120-150 minutes. The hot solution was filtered through hyflow bed and the bed was washed with 100 ml ethanol. The solution was filtered again through 0.2μ filter maintaining temperature at 70-75° C. The reaction mass was cooled to 15-20° C., stirred for an hour and filtered. The wet cake was washed with 100 ml of chilled ethanol and dried under vacuum at 40-45° C. to afford 89.5 gm of off white colored crystalline solid. to obtain clear solution The hot solution was filtered through hyflow bed the bed was washed with 100 ml ethanol The solution was filtered again through 0.2μ filter The reaction mass was cooled to 15-20° C. stirred for an hour filtered The wet cake was washed with 100 ml of chilled ethanol dried under vacuum at 40-45° C. to afford 89.5 gm of off white colored crystalline solid

反应条件: temp:72.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 100 gm of darunavir was dissolved in 1000 ml of denatured ethanol (mixture of 97% ethanol and 3% toluene) at 70-75° C. to obtain clear solution. 5 gm of activated charcoal was added and stirred for 120-150 minutes. The hot solution was filtered through hyflow bed and the bed was washed with 100 ml ethanol. The solution was filtered again through 0.2μ filter maintaining temperature at 70-75° C. The reaction mass was cooled to 15-20° C., stirred for an hour and filtered. The wet cake was washed with 100 ml of chilled ethanol and dried under vacuum at 40-45° C. to afford 89.5 gm of off white colored crystalline solid. to obtain clear solution The hot solution was filtered through hyflow bed the bed was washed with 100 ml ethanol The solution was filtered again through 0.2μ filter The reaction mass was cooled to 15-20° C. stirred for an hour filtered The wet cake was washed with 100 ml of chilled ethanol dried under vacuum at 40-45° C. to afford 89.5 gm of off white colored crystalline solid