反应 #2192308

反应方程式

1,1-dimethoxy-4-dimethylaminobut-3-en-2-one

2-Anilino-4-(6,7-dihydro-5H-pyrrolo[1,2-a]imidazol-3-yl)pyrimidine

phenyl guanidine bicarbonate

dimethylacetamide

→

title compound

收率 88.0%

2-Anilino-4-(dimethoxymethyl)pyrimidine

收率 88.0%

反应条件

后处理

1. 1
   温度to cool
2. 2
   其他the solvent removed by evaporation
3. 3
   workup.DISSOLUTIONThe residue was dissolved in EtOAc
4. 4
   洗涤the solution washed with water (×5), saturated sodium chloride (×2)
5. 5
   其他dried
6. 6
   其他evaporated

实验过程

A mixture of 1,1-dimethoxy-4-dimethylaminobut-3-en-2-one (Method 1; 20.0 g, 0.116 mol) and phenyl guanidine bicarbonate (25 g, 0.126 mol) in anhydrous dimethylacetamide (350 ml) was stirred and heated at 130° C. under nitrogen for 18 hours. The reaction mixture was allowed to cool and the solvent removed by evaporation. The residue was dissolved in EtOAc and the solution washed with water (×5), saturated sodium chloride (×2), dried and evaporated to give the title compound (24.7 g, 88%) as a dark brown oil. NMR: (CDCl3): 3.42 (s, 6H), 5.20 (s, 1H), 6.94 (d, 1H), 7.04 (t, 1H), 7.31 (m, 3H), 7.64 (d, 2H), 8.47 (d, 1H), m/z: 246.

来源