反应 #47935

反应方程式

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

2,3-dichloropyridine

N,N-diisopropylethylamine

→

desired compound

收率 26.0%

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

收率 26.0%

溶剂

dioxane N,N-dimethylacetamide

反应条件

后处理

1. 1
   其他The solvents were removed under vacuum
2. 2
   workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
3. 3
   洗涤washed with sat. NaHCO3 and brine
4. 4
   干燥The organic layer was dried over Na2SO4
5. 5
   过滤filtered
6. 6
   其他evaporated
7. 7
   其他to give a brown residue
8. 8
   其他The residue was purified

实验过程

N-(4-(Trifluoromethyl)phenyl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4-amine (700 mg, 3.4 mmol) was dissolved in a mixture of dioxane/N,N-dimethylacetamide (4:1) (2 mL). To the mixture was added 2,3-dichloropyridine (1.5 g, 10.2 mmol) and N,N-diisopropylethylamine (0.87 mL, 5.1 mmol). The mixture was heated in a sealed tube at 150° C. in a microwave (Emrys Optimizer model, Personal Chemistry) 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 using a gradient of ethyl acetate:hexane (0-100%) to give the desired compound as an off-white powder (340 mg, 26%).

来源