反应详情

A mixture of 64 (7.6 g, 0.035 mol) and POCl3 (100 ml) was heated at reflux for 5.5 hours. After stirring at room temperature overnight, the suspension was poured into saturated Na2CO3 and the mixture extracted with 20% CH3OH--CHCl3 (3×). The organic extracts were washed with saturated NaCl, dried, filtered and concentrated to dryness. The residue was chromatographed on silica gel and the product eluted with 5% CH3OH--CHCl3 to yield 5.0 g (71%) of 65; m.p. 219°-20° C. (CH3CN).

1. temperaturewas heated
2. temperatureat reflux for 5.5 hours
3. extractionthe mixture extracted with 20% CH3OH
4. washThe organic extracts were washed with saturated NaCl
5. customdried
6. filtrationfiltered
7. concentrationconcentrated to dryness
8. customThe residue was chromatographed on silica gel
9. washthe product eluted with 5% CH3OH