反应详情

200 mg (0.38 mmol) of 4-[6-((2S)-2-benzyloxycarbonylamino-2-tert-butoxycarbonyl-ethylamino)-purin-9-yl]-butyric acid ethyl ester was dissolved in 2 ml of dimethylformamide and 188 mg (1.9 mmol) of 1,4,5,6-tetrahydro-pyrimidin-2-ylamine was added. The solution was stirred at room temperature for 16 hours. The solvent was removed in vacuo, the residue was dissolved in dichloromethane and the solution was washed twice with 10% aqueous citric acid solution and twice with water. Product in the combined aqueous phase was extracted five times with dichloromethane. The combined organic phase was dried with sodium sulfate, filtered and the solvent was removed in vacuo. The residue was chromatographed on silica gel eluting with dichloromethane/methanol (10/1), followed by DCM/AcOH/water (85:15:1.5:1.5). Yield: 70.6 mg.

1. customThe solvent was removed in vacuo
2. dissolutionthe residue was dissolved in dichloromethane
3. washthe solution was washed twice with 10% aqueous citric acid solution and twice with water
4. extractionProduct in the combined aqueous phase was extracted five times with dichloromethane
5. dry with materialThe combined organic phase was dried with sodium sulfate
6. filtrationfiltered
7. customthe solvent was removed in vacuo
8. customThe residue was chromatographed on silica gel eluting with dichloromethane/methanol (10/1)