反应详情

温度

21 °C

To a stirred solution of 24 (70 mg, 0.144 mmol) in acetonitrile (0.42 mL) at 0° C. was added a solution of sodium dihydrogen phosphate (87 mg, 0.722 mmol) in water (0.17 mL). Then a solution of sodium chlorite (131 mg, 1.44 mmol) in water (0.59 mL) was added drop wise. The mixture was allowed to reach 21° C., stirring for 3 h at 21° C. The mixture was quenched with 1N NaOH, washed with CH2Cl2 (2×), and the combined organic phase was extracted with 1N NaOH. The combined aqueous phase was acidified to pH 1 with 1N HCl, extracted with AcOEt, dried (MgSO4) filtered and concentrated to afford 25 (59 mg, 88%) as a yellow solid. LRMS (ESI): calc. 462.1; found 485.2 (MNa)+.

1. customto reach 21° C.
2. customThe mixture was quenched with 1N NaOH
3. washwashed with CH2Cl2 (2×)
4. extractionthe combined organic phase was extracted with 1N NaOH
5. extractionextracted with AcOEt
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. concentrationconcentrated