反应详情

温度

55 °C

A mixture of tert-butyl 3,4-dihydroxypiperidine-1-carboxylate (300 mg, 1.38 mmol, 1 eq), 1,2-dichloroethane (6 mL) and TBAB (90 mg, 0.28 mmol, 0.2 eq) in 35% NaOH (10 mL) aqueous solution was heated at 55° C. for 72 h, then cooled to room temperature and extracted with CH2Cl2 (100 mL). The organic phase was washed with water (30 mL), dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by a silica gel column chromatography (20:1 (v/v) CH2Cl2/MeOH) to afford the title compound as pale yellow oil (250 mg, 75.00%). The compound was characterized by the following spectroscopic data: MS (ESI, pos. ion) m/z: 244.2 (M+1).

1. temperaturecooled to room temperature
2. extractionextracted with CH2Cl2 (100 mL)
3. washThe organic phase was washed with water (30 mL)
4. dry with materialdried over anhydrous Na2SO4
5. concentrationconcentrated in vacuo
6. customThe residue was purified by a silica gel column chromatography (20:1 (v/v) CH2Cl2/MeOH)