反应详情

To a solution of (S)-2,5-dihydro-1H-pyrrole-2-carboxylic acid (15 g, 133 mmol) and sodium hydroxide (10.6 g, 265 mmol) in THF (150 mL) cooled at 0° C. was added benzylchloroformate (32.0 mL, 166 mmol). The mixture was allowed to reach RT overnight. The reaction mixture was concentrated, water was added and the aqueous layer was extracted with Et2O (2×200 mL), acidified (6N HCl) and extracted with AcOEt (2×200 mL). The combined organic extracts were dried (Na2SO4), filtered and concentrated. The crude residue was used in the next step without purification. MS (UPLC/MS): 248 [M+H]+; tR (HPLC conditions b): 1.66 min.

1. concentrationThe reaction mixture was concentrated
2. additionwater was added
3. extractionthe aqueous layer was extracted with Et2O (2×200 mL)
4. extractionextracted with AcOEt (2×200 mL)
5. dry with materialThe combined organic extracts were dried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated
8. customThe crude residue was used in the next step without purification
9. custom1.66 min.