2-Amino-3-methylpyridine → 2-n-Propyl-3-ethoxycarbonyl-8-methylimidazo[1,2-a]pyridine
反応式
Cl[CH:2]([C:9](=O)[CH2:10][CH2:11]C)[CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5].[NH2:14][C:15]1[C:20]([CH3:21])=[CH:19][CH:18]=[CH:17][N:16]=1>C(O)CO.COC>[CH2:9]([C:2]1[N:14]=[C:15]2[C:20]([CH3:21])=[CH:19][CH:18]=[CH:17][N:16]2[C:3]=1[C:4]([O:6][CH2:7][CH3:8])=[O:5])[CH2:10][CH3:11]参加物
4
実験手順
2.3 g (11.9 mMol) of ethyl 2-chloro-3-oxo-hexane carboxylate and 2.6 g (23.8 mMol) of 2-amino-3-picoline are dissolved in 10 ml of ethyleneglycol-dimethylether and refluxed for 3 days. Then the solvent is evaporated off in vacuo and the residue is taken up in water/ethyl acetate 1:1. After the extraction the organic phase is separated off, washed with saturated saline solution, dried over magnesium sulphate and evaporated down. The residue is purified over a silica gel column (particle size: 0.063 to 0.02 mm), using as eluant mixtures of petroleum ether/ethyl acetate of increasing polarity (85:15, 80:20 and 1:1). The uniform fractions are evaporated down in vacuo.