反应详情

A solution of Example 9C (0.316 g, 0.90 mmol), 30% hydrogen peroxide (0.40 mL, 3.5 mmol), and lithium hydroxide monohydrate (0.076 g, 1.8 mmol) in 3:1 tetrahydrofuran/water (8 mL) was stirred at 0° C. for 3 hours and concentrated. The concentrate was dissolved in water and the pH adjusted to 10 with 1M NaOH. The solution was washed twice with diethyl ether, adjusted to pH 2 with 1M HCl, and extracted twice with ethyl acetate. The combined extracts were dried (MgSO4), filtered, and concentrated to provide the desired product. MS (ESI) m/e 324 (M+H)+.

1. concentrationconcentrated
2. dissolutionThe concentrate was dissolved in water
3. washThe solution was washed twice with diethyl ether
4. extractionextracted twice with ethyl acetate
5. dry with materialThe combined extracts were dried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated