反应详情

To a solution of (2S,3R)-3-azido-pyrrolidine-1,2-dicarboxylic acid 1-tert-butyl ester 2-methyl ester [361367-97-7] (210 mg, 0.777 mmol; Sunshine Ltd) in THF (6 mL) was added a solution of LiOH (55.8 mg, 2.33 mmol) in water (3 mL), followed by stirring at RT for 20 h. The reaction mixture was concentrated under reduced pressure and the residual aqueous phase was washed with EtOAc (3×). The water phase was adjusted to pH 2 to 3 by adding 1N aqueous HCl, followed by extraction with EtOAc (3×). The combined organics were dried (Phase separator) and concentrated in vacuo to give the crude title compound as a colorless oil. The crude product was used in the next reaction step without further purification. MS (LC/MS): 279 [M+Na]+, 200 [MH−tBu]+, 157 [MH−Boc]+; tR (HPLC conditions b): 2.77 min.

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. washthe residual aqueous phase was washed with EtOAc (3×)
3. additionby adding 1N aqueous HCl
4. extractionfollowed by extraction with EtOAc (3×)
5. customThe combined organics were dried (Phase separator)
6. concentrationconcentrated in vacuo