反应详情

In a 0.3-liter four-necked flask, 15.0 g (88.5 mmol) of 2-amino-6-chloropurine (manufactured by Sumika Fine Chemicals Co., Ltd.) and 26.9 g (194.6 mmol) of potassium carbonate were added to 195 ml of dimethylsulfoxide, and 8.0 g (442.5 mmol) of water was then added to the resulting mixture. The resulting mixture was stirred at room temperature. Next, 42.2 g (132.9 mmol) of diisopropyl 2,2,2-trichloroethylidenemalonate, which was prepared by the process described in U.S. Pat. No. 3,495,012, was added to the resulting mixture, and the mixture was stirred for two hours and a half at room temperature. Thereafter, the reaction mixture was filtered, and the filtrate was poured into water. The precipitated crystals were washed with 100 ml of water, collected by filtration, and then recrystallized from isopropyl alcohol, to give 27.1 g (60.1 mmol) of pale yellow crystals of 2-amino-6-chloro-9-(3,3-dicarboisopropoxy-2,2-dichlorocyclopropyl)purine. The yield was 67.9%.

1. additionwas then added to the resulting mixture
2. addition3,495,012, was added to the resulting mixture
3. stirringthe mixture was stirred for two hours
4. customat room temperature
5. filtrationThereafter, the reaction mixture was filtered
6. additionthe filtrate was poured into water
7. washThe precipitated crystals were washed with 100 ml of water
8. filtrationcollected by filtration
9. customrecrystallized from isopropyl alcohol