反应详情

To a solution of (2S,4S)-1-tert-butyl 2-methyl 4-aminopyrrolidine-1,2-dicarboxylate (4.6 g, 10.7 mmol) in CH2Cl2 (100 mL) were added 2,2,2-trichloroethyl carbonochloridate (1.73 mL, 12.88 mmol) and DIPEA (2.81 mL, 16.1 mmol). The reaction mixture was stirred at RT for 2 h then was poured into water. The desired compound was extracted with EtOAc (2×100 mL), the organic phases were joined, washed with 1N HCl then brine, dried over Na2SO4, filtered and concentrated. The crude residue was purified by flash column chromatography on silica gel (c-hexane to c-hexane/EtOAc 1:1). MS (UPLC): 421 [M+H]+, 419 [M−H]−; tR (HPLC conditions f): 1.11 min.

1. extractionThe desired compound was extracted with EtOAc (2×100 mL)
2. washwashed with 1N HCl
3. dry with materialbrine, dried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated
6. customThe crude residue was purified by flash column chromatography on silica gel (c-hexane to c-hexane/EtOAc 1:1)
7. custom1.11 min.