反应详情

[1,4]Diazepan-6-ol acetate (2B) (116 mg, 0.49 mmol) and 7-benzyl-8-chloro-1,3-dimethyl-3,7-dihydropurine-2,6-dione (100 mg, 0.33 mmol) were dissolved in 2-propanol (20 ml) and triethylamine (0.68 ml, 4.9 mmol) and the mixture was subjected to micro waves (150° C., 6 bar, 300 W, 8 hours). The solvents were evaporated and the remaining was redissolved in dichloromethane (20 ml) and water (20 ml). The aqueous layer was acidified with potassium hydrogen sulfate until pH=2. The aqueous layer was separated and aqueous sodium hydroxide was added until pH=12. The aqueous layer was extracted with 3×50 ml of dichloromethane, and the combined organic material were added excess trifluoroacetic acid, and evaporated, to afford 123 mg of the title compound as a brown oil in 75% yield.

1. customwas subjected to micro waves (150° C., 6 bar, 300 W, 8 hours)
2. customThe solvents were evaporated
3. dissolutionthe remaining was redissolved in dichloromethane (20 ml)
4. customThe aqueous layer was separated
5. additionaqueous sodium hydroxide was added until pH=12
6. extractionThe aqueous layer was extracted with 3×50 ml of dichloromethane
7. additionthe combined organic material were added excess trifluoroacetic acid
8. customevaporated