반응 #2030970

반응 방정식

8-chloro-7-(2-propen-1-yl)-3,7-dihydro-1H-purine-2,6-dione

sodium carbonate

4-bromo-1,1,1-trifluorobutane

→

8-chloro-7-(2-propen-1-yl)-3-(4,4,4-trifluorobutyl)-3,7-dihydro-1H-purine-2,6-dione

수율 57.0%

용매

dimethylformamide

반응 조건

후처리

1. 1
   기타The reaction mixture was partitioned between ethyl acetate and water
2. 2
   기타The organic phase was separated
3. 3
   세척washed with hydrochloric acid (2N), brine
4. 4
   건조dried (MgSO4)
5. 5
   기타evaporated to dryness
6. 6
   기타The crude product was triturated with ether
7. 7
   여과the solid collected by filtration

실험 절차

8-chloro-7-(2-propen-1-yl)-3,7-dihydro-1H-purine-2,6-dione (1.5 g, 6.64 mmol), sodium carbonate (844 mg, 7.9 mmol) and 4-bromo-1,1,1-trifluorobutane (1.39 g, 7.3 mmol) were stirred in dimethylformamide (25 ml, dry) for seven days. The reaction mixture was partitioned between ethyl acetate and water. The organic phase was separated and washed with hydrochloric acid (2N), brine, dried (MgSO4) and then evaporated to dryness. The crude product was triturated with ether and the solid collected by filtration to afford 8-chloro-7-(2-propen-1-yl)-3-(4,4,4-trifluorobutyl)-3,7-dihydro-1H-purine-2,6-dione as a white solid (1.23 g, 57%). m/z 337 [MH+].

출처