反应详情

温度

100 °C

Into a sealed tube were added 4-amino-2-chloro-pyrimidine-5-carbonitrile (837 mg, 5.4 mmol), sodium azide (7.1 mmol, 1.3 eq.), triethylamine hydrochloride (7.1 mmol, 1.3 eq.) and 14 mL of toluene. The tube was tightly capped and the reaction was stirred and heated to 100° C. overnight. The mixture was cooled to room temperature, diluted with ethyl acetate, transferred to a separatory funnel and extracted three times with water. The aqueous extractions were combined and acidified to a pH of 4 with concentrated HCl. The precipitate was collected by filtration, washed with acetonitrile, and dried under vacuum to afford 460 mg of the product, which was used without further purification. MS (EI) for C5HClN7: 198 (M+H).

1. customThe tube was tightly capped
2. temperatureThe mixture was cooled to room temperature
3. customtransferred to a separatory funnel
4. extractionextracted three times with water
5. extractionThe aqueous extractions
6. filtrationThe precipitate was collected by filtration
7. washwashed with acetonitrile
8. customdried under vacuum