反应详情

温度

70 °C

A solution of 2-amino-6-chloropurine (4.6 g, 27.5 mmole) and cyclopropylamine (12.5 g, 220 mmole 8 equiv) in MeOH (100 ml) was heated at 50° C. for 18 hours. Then 2-methoxyethanol (50 ml) was added, and the reaction was heated at 70° C. for an additional 6 hours. After cooling, a small amount of unreacted starting material was filtered off, and the filtrate was evaporated and purified on a silica gel column eluting with CHCl3 : 5% to 10% MeOH. The product was then recrystallised twice from MeOH and once from EtOH as a hydrochloride salt to give 1.45 g, (23%) of product; m.p. 253°-257° C.,

1. temperatureAfter cooling
2. filtrationwas filtered off
3. customthe filtrate was evaporated
4. custompurified on a silica gel column
5. washeluting with CHCl3
6. customThe product was then recrystallised twice from MeOH and once from EtOH as a hydrochloride salt