反应详情

A mixture of Example 126D (12.5 g, 31.5 mmol) in dioxane (400 mL) and H2O (400 mL) had a solution of Na2SO3 (43.7 g, 347 mmol) in H2O (400 mL) added and was heated to reflux for 21 hours. The mixture was concentrated to half volume and extracted with CH2Cl2 (3×200 mL). The organic was then washed with brine, dried (MgSO4), filtered and concentrated. Purification by trituration (CH2Cl2, tBuOMe, and Hexanes) afforded 5.2 g (52%) of the title compound. MS (ESI) m/z 317 (M+H)+.

1. additionadded
2. temperaturewas heated
3. temperatureto reflux for 21 hours
4. concentrationThe mixture was concentrated to half volume
5. extractionextracted with CH2Cl2 (3×200 mL)
6. washThe organic was then washed with brine
7. dry with materialdried (MgSO4)
8. filtrationfiltered
9. concentrationconcentrated
10. customPurification by trituration (CH2Cl2, tBuOMe, and Hexanes)