反应详情

To tert-butyl 4-hydroxy-2-(4-methyl-5-oxo-2,5-dihydrofuran-3-yl)-1-oxo-2,8-diazaspiro[4.5]decane-8-carboxylate (see example I-37A and I-37B, Step C, racemate prior to chiral HPLC separation) (200 mg, 0.546 mmol) in DCM (2.8 mL) was added sodium bicarbonate (68.8 mg, 0.819 mmol) and Dess-Martin periodinane (347 mg, 0.819 mmol). The reaction mixture was vigorously stirred for 1.5 h, then quenched with 10% Na2S2O3 and NaHCO3 aqueous solutions, and stirred for 20 min. The aqueous layer was extracted with DCM, and the organic layers were washed with brine, dried, and concentrated to give tert-butyl 2-(4-methyl-5-oxo-2,5-dihydrofuran-3-yl)-1,4-dioxo-2,8-diazaspiro[4.5]decane-8-carboxylate. LC/MS: [(M+1)]+=365

1. customand I-37B, Step C, racemate prior to chiral HPLC separation) (200 mg, 0.546 mmol) in DCM (2.8 mL)
2. customquenched with 10% Na2S2O3 and NaHCO3 aqueous solutions
3. stirringstirred for 20 min
4. extractionThe aqueous layer was extracted with DCM
5. washthe organic layers were washed with brine
6. customdried
7. concentrationconcentrated