反应详情

温度

80 °C

A mixture of the compound of Example 2 (410 mg, 0.58 mmole) and SnCl2, 2H2O (1.32 g, 5.8 mmoles) in AcOEt (10 ml) is heated at 80° C. for 90 minutes. The reaction medium is then cooled down to 0° C. before being poured into a saturated aqueous solution of Na2CO3 (40 ml). The heterogeneous mixture thus obtained is filtered on celite and rinsed with AcOEt (2×50 ml). After decantation, the organic phases are combined, dried over Na2SO4, filtered and the solvent is evaporated off under reduced pressure. The residue obtained is taken up in a mixture of heptane/AcOEt in order to produce a white solid, after filtration, with a yield of 78% (290 mg). Melting point: 108-109° C.

1. temperatureThe reaction medium is then cooled down to 0° C.
2. customThe heterogeneous mixture thus obtained
3. filtrationis filtered on celite
4. washrinsed with AcOEt (2×50 ml)
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. customthe solvent is evaporated off under reduced pressure
8. customThe residue obtained
9. customto produce a white solid
10. filtrationafter filtration