反应详情

温度

110 °C

Compound of formula (23) (3.16 g, 8.84 mmol), prepared according to example 4, was dissolved in ammonia-saturated ethanol (40 ml, containing approximately 160 mmol ammonia) and heated to 110° C. for 3 h. The mixture was then evaporated to dryness, and the residue was mixed with an aqueous, saturated solution of NaHCO3 (20 ml). The mixture was extracted with toluene (2×20 ml), and the combined extracts were washed with water (2×20 ml). The combined extracts were then extracted with 10% aqueous HCl (3×20 ml), and the combined acidic extracts were basified with gaseous ammonia, and extracted with toluene (2×20 ml). The combined organic extracts were dried over Na2SO4, and concentrated under reduced pressure, to yield compound of formula (XX) (1.57 g, 89%).

1. customThe mixture was then evaporated to dryness
2. additionthe residue was mixed with an aqueous, saturated solution of NaHCO3 (20 ml)
3. extractionThe mixture was extracted with toluene (2×20 ml)
4. washthe combined extracts were washed with water (2×20 ml)
5. extractionThe combined extracts were then extracted with 10% aqueous HCl (3×20 ml)
6. extractionextracted with toluene (2×20 ml)
7. dry with materialThe combined organic extracts were dried over Na2SO4
8. concentrationconcentrated under reduced pressure