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 (Water's sunfire column) eluting with a gradient of acetonitrile in 0.1% aqueous trifluoroacetic acid. Fractions containing product were evaporated to remove acetonitrile, neutralised with saturated sodium bicarbonate and extracted with dichloromethane which was dried over magnesium sulfate and evaporated to afford the titled compound (110 mg).

1. customThe mixture was evaporated to dryness
2. dissolutiondissolved in methanol (4 mL)
3. custompurified on reverse phase HPLC (Water's sunfire column)
4. washeluting with a gradient of acetonitrile in 0.1% aqueous trifluoroacetic acid
5. additionFractions containing product
6. customwere evaporated
7. customto remove acetonitrile
8. extractionextracted with dichloromethane which
9. dry with materialwas dried over magnesium sulfate
10. customevaporated