反应详情

Methyl 4-(Boc-amino)pyridine-3-carboxylate (2.38 g, 9.4 mmol) was dissolved in TFA (20 mL) and the solution was allowed to stir for 45 min. The solvent was removed in vacuo and the residue was partitioned between 25% isopropanol in chloroform and satd aq sodium bicarbonate. The layers were separated and the aqueous phase was extracted again with 25% isopropanol in chloroform. The combined organic extracts were dried (MgSO4), filtered and concentrated in vacuo to give a solid which was washed with diisopropyl ether and dried in vacuo to give the title compound (1.327 g, 92%) as an off-white solid.

1. customThe solvent was removed in vacuo
2. customthe residue was partitioned between 25% isopropanol in chloroform
3. customThe layers were separated
4. extractionthe aqueous phase was extracted again with 25% isopropanol in chloroform
5. dry with materialThe combined organic extracts were dried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customto give a solid which
9. washwas washed with diisopropyl ether
10. customdried in vacuo