反应详情

A solution of 4-cyano-1H-imidazole-2-carboxylic acid[2-(4,4-dimethyl-cyclohex-1-enyl)-6-(2,2,6,6-tetramethyl-tetrahydro-pyran-4-yl)-pyridin-3-yl]-amide (50.0 mg, 0.108 mmol, as prepared in Example 15, step (h)) in EtOH (2 mL) was treated with methanesulfonic acid (7.0 μL, 0.108 mmol) at room temperature for 1 h. The solvents were evaporated in vacuo, and the residue was dried under high vacuum overnight. The solid was dissolved in a minimum amount of EtOH (2 mL) with sonication and heating. While warm, the solution was slowly treated with hexanes (3 mL) to the cloud point. The mixture was heated again until clear, the sides of the vial were scratched, and the mixture was allowed to cool. The solid was filtered and air-dried to afford the title compound (24 mg, 40%) as white crystals. Mass spectrum (APCI, m/z): Calcd. for C27H35N5O2, 462.3 (M+H), found 462.3.

1. customThe solvents were evaporated in vacuo
2. customthe residue was dried under high vacuum overnight
3. dissolutionThe solid was dissolved in a minimum amount of EtOH (2 mL) with sonication
4. temperatureheating
5. temperatureWhile warm
6. additionthe solution was slowly treated with hexanes (3 mL) to the cloud point
7. temperatureThe mixture was heated again until clear, the sides of the
8. temperatureto cool
9. filtrationThe solid was filtered
10. customair-dried