反应详情

温度

80 °C

The product from Example 228d (0.250 g, 1.71 mmol) was combined with phosphorous oxychloride (4 mL) and heated under a nitrogen atmosphere at 80° C. for 18.5 h followed by vacuum distillation to remove the volatiles. The residue was slurried with ice and made basic (pH 7-8) with concentrated ammonium hydroxide. The title compound was collected by vacuum filtration, water washed and dried under vacuum to give a gray solid (0.245 g, 87%) sufficiently pure for use as isolated.

1. distillationfollowed by vacuum distillation
2. customto remove the volatiles
3. filtrationThe title compound was collected by vacuum filtration, water
4. washwashed
5. customdried under vacuum