反应详情

温度

50 °C

To (S)-tert-butyl 4-(1-cyano-2-(4′-(isopropylsulfonyl)biphenyl-4-yl)ethylcarbamoyl)tetrahydro-2H-pyran-4-ylcarbamate (Example 4, step (ii(ii)), 300 mg) was added formic acid (4 mL) and the mixture heated to 50° C. for 20 min. The mixture was evaporated to dryness, dissolved in methanol (10 mL), re-evaporated to dryness, dissolved in methanol (6 mL) and purified on reverse phase HPLC eluting with 25 to 95% methanol in 0.1% aqueous TFA on a Waters SunFire column. The material was converted to free base by evaporating the relevant fractions, dissolving in dichloromethane (20 mL) and shaking with saturated sodium bicarbonate solution (20 mL). The dichloromethane was dried and evaporated to afford the titled compound (67 mg).

1. customThe mixture was evaporated to dryness
2. dissolutiondissolved in methanol (10 mL)
3. customre-evaporated to dryness
4. dissolutiondissolved in methanol (6 mL)
5. custompurified on reverse phase HPLC
6. washeluting with 25 to 95% methanol in 0.1% aqueous TFA on a Waters SunFire column
7. customby evaporating the relevant fractions
8. dissolutiondissolving in dichloromethane (20 mL)
9. dry with materialThe dichloromethane was dried
10. customevaporated