反应详情

(S)-tert-Butyl 4-(1-cyano-2-(4′-methoxybiphenyl-4-yl)ethylcarbamoyl)tetrahydro-2H-pyran-4-ylcarbamate (Example 20, step (i), 120 mg) was dissolved in formic acid (3 mL) and the mixture stirred at room temperature for 3 h. The mixture was evaporated to dryness, dissolved in methanol (10 mL), re-evaporated to dryness, dissolved in methanol (5.5 mL) and purified on reversed phase HPLC eluting with methanol in 0.1% aqueous TFA on a Water's SunFire column. The material was converted to free base by evaporating the relevant fractions, dissolving in ethyl acetate (20 mL) and extracted with saturated sodium bicarbonate solution (20 mL). The sodium bicarbonate solution was further extracted with ethyl acetate (20 mL). The combined ethyl acetate extracts were dried and evaporated to afford the titled compound (91 mg).

1. customThe mixture was evaporated to dryness
2. dissolutiondissolved in methanol (10 mL)
3. customre-evaporated to dryness
4. dissolutiondissolved in methanol (5.5 mL)
5. custompurified on reversed phase HPLC
6. washeluting with methanol in 0.1% aqueous TFA on a Water's SunFire column
7. customby evaporating the relevant fractions
8. dissolutiondissolving in ethyl acetate (20 mL)
9. extractionextracted with saturated sodium bicarbonate solution (20 mL)
10. extractionThe sodium bicarbonate solution was further extracted with ethyl acetate (20 mL)
11. dry with materialThe combined ethyl acetate extracts were dried
12. customevaporated