反应详情

Trifluoroacetic Acid (1 mL) was added to a solution of tert-butyl 4-({2-(3-{[tert-butyl(dimethyl)silyl]oxy}-2,2-dimethylpropyl)-6-[5-(cyclopropylcarbamoyl)-3-fluoro-2-methylphenyl]-1-oxo-1,2-dihydroisoquinolin-4-yl}sulfanyl)piperidine-1-carboxylate (Example 58d, 0.123 g) in DCM (3 mL). The reaction was stirred at room temperature for 30 min. Toluene (5 mL) was added and the volatiles were removed under reduced pressure. The residue was dissolved in MeOH (1 mL)/DMF (1 mL) and purified by preparative HPLC (Xbridge column using a 95-5% gradient of 0.2% aqueous ammonia in acetonitrile) and after solvent removal, the residue was triturated with diethyl ether. This was dissolved in methanol and purified by preparative HPLC (Sunfire C18 column using a 95-30% gradient of 0.1% aqueous formic acid in methanol run over 16 min). The relevant fractions were lyophilized before the solid was dissolved in methanol and passed through a Stratospheres PL-HCO3 cartridge. The solvent was removed from the resulting filtrate under reduced pressure to give, after trituration with diethyl ether, the title compound (0.035 g).

1. customthe volatiles were removed under reduced pressure
2. dissolutionThe residue was dissolved in MeOH (1 mL)/DMF (1 mL)
3. custompurified by preparative HPLC (Xbridge column
4. customafter solvent removal
5. customthe residue was triturated with diethyl ether
6. dissolutionThis was dissolved in methanol
7. custompurified by preparative HPLC (Sunfire C18 column
8. waitrun over 16 min
9. dissolutionwas dissolved in methanol
10. customThe solvent was removed from the resulting filtrate under reduced pressure
11. customto give