반응 #47905

반응 방정식

N-(4-Fluorophenyl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4-amine

2,3-dichloropyridine

N,N-diisopropylethylamine

→

desired compound

수율 30.0%

6-(3-Chloropyridin-2-yl)-N-(4-fluorophenyl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4-amine

수율 30.0%

용매

dioxane N,N-dimethylacetamide

반응 조건

후처리

1. 1
   기타The solvents were removed under vacuum
2. 2
   workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
3. 3
   세척washed with sat. NaHCO3 and brine
4. 4
   건조The organic layer was dried over Na2SO4
5. 5
   여과filtered
6. 6
   기타evaporated
7. 7
   기타to give a brown residue
8. 8
   기타The residue was purified by silica gel chromatography

실험 절차

N-(4-Fluorophenyl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4-amine (0.47 g, 1.92 mmol) was dissolved in a mixture of dioxane/N,N-dimethylacetamide (4:1) (3 mL). To the mixture was added 2,3-dichloropyridine (420 mg, 2.86 mmol) and N,N-diisopropylethylamine (0.38 mL, 2.2 mmol). The mixture was heated at 150° C. in a Personal Chemistry microwave for 16 h. The solvents were removed under vacuum and the residue was dissolved in ethyl acetate and washed with sat. NaHCO3 and brine. The organic layer was dried over Na2SO4, filtered and evaporated to give a brown residue. The residue was purified by silica gel chromatography using a gradient of ethyl acetate:hexane (0-100%) to give the desired compound as an off-white powder (200 mg, 30%).

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