反应详情

A mixture of the product of part (i) (6.4 g, 45 mmol) and phosphoryl chloride (30 ml) was heated under reflux for 3 hours. The excess phosphoryl chloride was removed by distillation under reduced pressure and the residue was poured into ice-water. The resulting mixture was extracted with methylene chloride (3×50 ml) and the combined organic extracts were washed with water and dried over magnesium sulphate. The solvent was removed under reduced pressure and the resulting oil was distilled under reduced pressure to provide the title compound (4.81 g, 66%), b.p. 74° C. at 22 mm Hg, which was characterised by 1H-NMR spectroscopy.

1. temperaturewas heated
2. temperatureunder reflux for 3 hours
3. customThe excess phosphoryl chloride was removed by distillation under reduced pressure
4. additionthe residue was poured into ice-water
5. extractionThe resulting mixture was extracted with methylene chloride (3×50 ml)
6. washthe combined organic extracts were washed with water
7. dry with materialdried over magnesium sulphate
8. customThe solvent was removed under reduced pressure
9. distillationthe resulting oil was distilled under reduced pressure