反应详情

温度

50 °C

To (S)-tert-butyl 4-(1-cyano-2-(4-(2-methyl-1-oxoisoindolin-5-yl)phenyl)ethylcarbamoyl)tetrahydro-2H-pyran-4-ylcarbamate (Example 31, step (v), 436 mg) was added formic acid (9.7 mL) and the mixture heated to 50° C. for 15 min. The mixture was allowed to cool to room temperature, diluted with methanol and then evaporated to dryness. The material was purified by reversed phase HPLC (Waters X-Bridge column) eluting with methanol in aqueous 0.1% trifluoroacetic acid as eluent. The fractions containing the desired compound were combined, evaporated and then dissolved in dichloromethane and washed with saturated aqueous sodium hydrogen carbonate. The organic layer was dried over magnesium sulfate and evaporated. The residue was triturated with diethyl ether and evaporated to give a product that was slurried in water (6.9 mL) and acetonitrile (0.36 mL) for 4 days. The solid was collected by filtration, washed with water and then dried under vacuum at 50° C. to afford the titled compound (212 mg).

1. temperatureto cool to room temperature
2. customevaporated to dryness
3. customThe material was purified by reversed phase HPLC (Waters X-Bridge column)
4. washeluting with methanol in aqueous 0.1% trifluoroacetic acid as eluent
5. additionThe fractions containing the desired compound
6. customevaporated
7. dissolutiondissolved in dichloromethane
8. washwashed with saturated aqueous sodium hydrogen carbonate
9. dry with materialThe organic layer was dried over magnesium sulfate
10. customevaporated
11. customThe residue was triturated with diethyl ether
12. customevaporated
13. customto give a product that
14. filtrationThe solid was collected by filtration
15. washwashed with water
16. customdried under vacuum at 50° C.