反应详情

温度

50 °C

To (S)-tert-butyl 4-(1-cyano-2-(4′-cyanobiphenyl-4-yl)ethylcarbamoyl)tetrahydro-2H-pyran-4-ylcarbamate (Example 3, step (v), 420 mg) was added formic acid (2 mL) and the mixture heated to 50° C. for 10 min. The mixture was evaporated to dryness, dissolved in methanol (4 mL) and purified on reverse phase HPLC eluting with 25 to 85% acetonitrile in 0.1% TFA on a Water's Sunfire column. Fractions containing product were evaporated to remove acetonitrile, neutralised with saturated sodium bicarbonate and extracted with dichloromethane which was dried and evaporated to afford the titled compound as a solid (110 mg).

1. customThe mixture was evaporated to dryness
2. dissolutiondissolved in methanol (4 mL)
3. custompurified on reverse phase HPLC
4. washeluting with 25 to 85% acetonitrile in 0.1% TFA on a Water's Sunfire column
5. additionFractions containing product
6. customwere evaporated
7. customto remove acetonitrile
8. extractionextracted with dichloromethane which
9. customwas dried
10. customevaporated