反应详情

To a solution of (2S,3R)-3-Hydroxy-2-methylpyrrolidine-1,2-dicarboxylic acid 1-tert-butyl ester-2-methyl ester (25A) (362 mg, 1.39 mmol) in CH2Cl2 (4 mL) was added imidazole (284 mg, 4.17 mmol) then tert-butydimethylsilyl chloride (1.05 g, 6.95 mmol). After stirring overnight, the reaction was partitioned between H2O and CH2Cl2. The CH2Cl2 layer was washed with 1M H3PO4 (2×) and brine, dried (MgSO4), then filtered and concentrated under reduced pressure. The residue was chromatographed (silica gel) eluting with 30% EtOAc/hexane to yield the title compound (456 mg) as a white solid.

1. customthe reaction was partitioned between H2O and CH2Cl2
2. washThe CH2Cl2 layer was washed with 1M H3PO4 (2×) and brine
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThe residue was chromatographed (silica gel)
7. washeluting with 30% EtOAc/hexane