反应详情

温度

0 °C

To a stirred solution of triphosgene (2.08 g, 7.04 mmol) in THF (10 mL) at room temperature under argon was added a suspension of 4-(4-chlorophenyl)-6-hydrazinyl-2-(methylthio)-5-phenylpyrimidine (3.52 mmol) in THF (5 mL). The reaction mixture was stirred overnight. Analysis by HPLC/MS indicated that no starting material remained. The reaction mixture was cooled to 0° C. in an ice bath and ice water (50 mL) was added. After stirring for 30 min, the solid precipitate was collected and further washed with water (50 mL). After drying, the title compound (1.25 g) was obtained as an off-white solid. HPLC/MS: retention time=3.51 min, [M+H]30 =369.

1. stirringAfter stirring for 30 min
2. customthe solid precipitate was collected
3. washfurther washed with water (50 mL)
4. customAfter drying