تفاعل #47905

معادلة التفاعل

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

2,3-dichloropyridine

N,N-diisopropylethylamine

→

desired compound

المردود 30.0%

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

المردود 30.0%

المذيبات

dioxane N,N-dimethylacetamide

ظروف التفاعل

المعالجة

1. 1
   أخرىThe solvents were removed under vacuum
2. 2
   workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
3. 3
   غسيلwashed with sat. NaHCO3 and brine
4. 4
   تجفيفThe organic layer was dried over Na2SO4
5. 5
   ترشيحfiltered
6. 6
   أخرىevaporated
7. 7
   أخرىto give a brown residue
8. 8
   أخرىThe residue was purified by silica gel chromatography

الإجراء التجريبي

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%).

المصدر