反应详情

A mixture of intermediate (53) (0.010 mol) in methanol (150 ml) was hydrogenated at 50° C. with palladium-on-carbon (10%, 1 g) as a catalyst. After uptake of hydrogen (2 equivalents), the catalyst was filtered off and the filtrate was evaporated. Toluene was added and azeotroped on the rotary evaporator. The residue was dried over the weekend under a gentle stream of nitrogen. Toluene was added and azeotroped on the rotary evaporator. The residue was stirred in DCM (50 ml). NaOCH3 (0.504 g) was added and the reaction mixture was stirred for one hour under nitrogen. More methanol (25 ml) was added and the mixture was stirred for 30 minutes. The precipitate was filtered off and the filtrate was evaporated in vacuo, yielding 1.54 g of 1-(3-aminopropyl)dihydro-2,4(1H,3H)-pyrimidinedione (intermediate 54).

1. customthe filtrate was evaporated
2. additionToluene was added
3. customazeotroped on the rotary evaporator
4. customThe residue was dried over the weekend under a gentle stream of nitrogen
5. additionToluene was added
6. customazeotroped on the rotary evaporator
7. additionNaOCH3 (0.504 g) was added
8. stirringthe reaction mixture was stirred for one hour under nitrogen
9. additionMore methanol (25 ml) was added
10. stirringthe mixture was stirred for 30 minutes
11. filtrationThe precipitate was filtered off
12. customthe filtrate was evaporated in vacuo