反应详情

温度

120 °C

A mixture of compound D5 (2.3 g, 9.77 mmol) and phosphorus(V) oxychloride (50 ml) was heated at 120° C. for 5 h. After cooling to room temperature the solvents were evaporated in vacuo. The residue thus obtained was carefully poured into a mixture of crushed ice and NaHCO3 (aqueous sat. solution). Then EtOAc was added and the mixture was stirred for 2 h. until complete hydrolysis of the remaining phosphorus oxychloride had occurred. The organic layer was then separated, washed with brine, dried (Na2SO4) and the solvent evaporated in vacuo to give a residue that forms a precipitate upon the addition of Et2O. The solid was filtered off and dried in vacuo to yield compound D6 (0.82 g, 33%) as yellow solid.

1. temperatureAfter cooling to room temperature the solvents
2. customwere evaporated in vacuo
3. customThe residue thus obtained
4. customThe organic layer was then separated
5. washwashed with brine
6. dry with materialdried (Na2SO4)
7. customthe solvent evaporated in vacuo
8. customto give a residue that
9. filtrationThe solid was filtered off
10. customdried in vacuo