反应详情

Stir a solution of 3-(4-bromo-benzoyl)-pyrrolidine-1-carboxylic acid tert-butyl ester (3.79 g, 10.7 mmol) in 4 M HCl in dioxane (21.4 mL) at 0° C. for one hour. 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 chromatograph, eluting with 5-10% in MeOH (2N NH3)/CH2Cl2 to give 2.24 g (82%) of the title compound. LC-MS m/z (79Br) 254.0 [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 chromatograph
10. washeluting with 5-10% in MeOH (2N NH3)/CH2Cl2