反应详情

Orvepitant Hydrochloride (1.00 G) Was Suspended In Ethyl Acetate (20 Ml) And Water (10 ml) and 25% w/w ammonia (10 ml) were added. The aqueous layer was separated and the organic layer was washed with 10% w/w sodium chloride solution (2×10 ml). The organic solution was separated, evaporated to dryness and isopropanol (20 ml) was added. The solution was evaporated to dryness. The material was diluted with isopropanol (6 ml) and a solution of maleic acid (0.174 g) in isopropanol (2.0 ml) was added. Iso-octane (a total of 8 ml) was added and the solution was stirred overnight. The solution was evaporated to an oil. Tert-butyl methyl ether (10 ml) was added and the solution was evaporated to dryness. Repeat the addition of tert-butyl methyl ether and evaporation a total of 4 times. On final evaporation, a foam forms that solidifies to give the title compound.

1. customThe aqueous layer was separated
2. washthe organic layer was washed with 10% w/w sodium chloride solution (2×10 ml)
3. customThe organic solution was separated
4. customevaporated to dryness and isopropanol (20 ml)
5. additionwas added
6. customThe solution was evaporated to dryness
7. additionThe material was diluted with isopropanol (6 ml)
8. additiona solution of maleic acid (0.174 g) in isopropanol (2.0 ml) was added
9. additionIso-octane (a total of 8 ml) was added
10. customThe solution was evaporated to an oil
11. additionTert-butyl methyl ether (10 ml) was added
12. customthe solution was evaporated to dryness
13. additionRepeat the addition of tert-butyl methyl ether and evaporation a total of 4 times
14. customOn final evaporation