反应 #1914857

反应方程式

1-6

2-Oxo-6-(5,6,7,8-tetrahydro-[1,8]-naphthyridin-2-yl)-hexyl-phosphonic acid dimethyl ester

5-formyl-2-methylpyrimidine

K2CO3

→

1-7

1-(2-Methyl-pyrimidin-5-yl)-7-(5,6,7,8-tetrahydro-[1,8]naphthyridin-2-yl)-hept-1-en-3-one

溶剂

DMF

反应条件

后处理

1. 1
   浓缩concentrated to a paste
2. 2
   workup.ADDITIONThe residue was diluted with water
3. 3
   萃取extracted with ethyl acetate
4. 4
   干燥dried over magnesium sulfate
5. 5
   浓缩concentration
6. 6
   其他the residue was chromatographed on silica gel (70 chloroform/25 ethyl acetate/5 methanol)

实验过程

To a solution of 1-6 (5.5 g, 16.2 mmol), 5-formyl-2-methylpyrimidine (1-6a, 1.8 g, 14.7 mmol; for preparation, see J. Heterocyclic Chem., 28, 1281 (1991)) in 40 mL DMF was added K2CO3 (4.07 g, 32 mmol). The mixture was stirred at ambient temperature for 15 hr, and concentrated to a paste. The residue was diluted with water, extracted with ethyl acetate, and dried over magnesium sulfate. Following concentration, the residue was chromatographed on silica gel (70 chloroform/25 ethyl acetate/5 methanol) to give 1-7 as a white solid.

来源