反应详情

To a stirred solution of triphosgene (2.86 g, 9.66 mmol) in THF (10 mL) at room temperature under argon was added a suspension of 4-(4-chlorophenyl)-6-hydrazinylpyrimidine (825 mg, 3.22 mmol) in THF (10 mL). The reaction mixture was stirred overnight. Analysis by HPLC/MS indicated that no starting material remained. Solvent was removed under reduced pressure and water (50 mL) was added. After stirring for 30 min, the solid precipitate was collected and further washed with water (3×10 mL), then methanol (3×5 mL). The title compound (793 mg) was obtained as an off-white solid. HPLC/MS: retention time=2.74 min, [M+H]30 =247.

1. customSolvent was removed under reduced pressure and water (50 mL)
2. additionwas added
3. stirringAfter stirring for 30 min
4. customthe solid precipitate was collected
5. washfurther washed with water (3×10 mL)