反应详情

温度

55 °C

40 g of Bosentan sodium salt were dissolved in acetone (353 g) and 8.48 g of hydrochloridric acid were added. Precipitated salts were filtered off and the clear solution was concentrated by distillation to a residual volume of 190 mL. The mixture was cooled to 55° C. and demineralized water (58 g) was slowly dropped keeping the temperature at 55° C. After 2 hours aging the temperature was decreased to 20° C. in 1 hour and stirred for additional 2 hours at that temperature. The precipitated solid was collected by filtration and the cake was washed with water-acetone 1:1 (38 g). 39.4 g of the desired product were obtained after drying in vacuo.

1. filtrationPrecipitated salts were filtered off
2. concentrationthe clear solution was concentrated by distillation to a residual volume of 190 mL
3. additiondemineralized water (58 g) was slowly dropped
4. customat 55° C
5. waitthe temperature was decreased to 20° C. in 1 hour
6. filtrationThe precipitated solid was collected by filtration
7. washthe cake was washed with water-acetone 1:1 (38 g)