反应详情

CH2Cl2 (10 ml) was added to the HNO3/H2SO4 mixture, and the resulting solution was stirred for 15 minutes. Potassium 4-(hydroxy)butanoate (500 mg, 3.52 mmol) was then added in small portions to the methylenechloride solution kept at 0-5° C. The mixture was kept under stirring for 6 hours while the temperature was allowed to reach 25° C. gradually. Water (50 ml) was added to the reaction mixture and the resulting mixture was extracted with CH2Cl2 (3×25 ml). The combined organic phases were washed with water, dried over MgSO4 and concentrated to dryness under reduced pressure. 4-(Nitrooxy)butanoic acid was obtained as a yellow oil (300 mg, 57%) and used in the next step.

1. customkept at 0-5° C
2. stirringunder stirring for 6 hours while the temperature
3. customto reach 25° C.
4. extractionthe resulting mixture was extracted with CH2Cl2 (3×25 ml)
5. washThe combined organic phases were washed with water
6. dry with materialdried over MgSO4
7. concentrationconcentrated to dryness under reduced pressure