反应详情

Stir a solution of 3-(5-bromo-pyridine-2-carbonyl)-pyrrolidine-1-carboxylic acid tert-butyl ester (0.65 g, 1.8 mmol) in 4 M HCl in dioxane (3.7 mL) at 0° C. for 1 h. Concentrate the reaction mixture, dilute the mixture with CH2Cl2, wash with 5 N NaOH (15 mL), and back-extract the aqueous with CH2Cl2. Wash the combined organic layer with brine, dry over Na2SO4, filter and concentrate. Purify the crude material by flash chromatography, eluting with 10% MeOH (2N NH3)/CH2Cl2 to give 0.4 g (85%) of the title compound. LC-MS/ES m/z (81Br) 257.0 [M+H]+.

1. concentrationConcentrate the reaction mixture
2. additiondilute the mixture with CH2Cl2
3. washwash with 5 N NaOH (15 mL)
4. extractionback-extract the aqueous with CH2Cl2
5. washWash the combined organic layer with brine
6. dry with materialdry over Na2SO4
7. filtrationfilter
8. concentrationconcentrate
9. customPurify the crude material by flash chromatography
10. washeluting with 10% MeOH (2N NH3)/CH2Cl2