Dimethylamine → Methyl (dimethylamino)(oxo)acetate
反応式
[CH3:1][NH:2][CH3:3].C[O-].[Na+].[C:7]([O:13]C)(=O)[C:8]([O:10][CH3:11])=[O:9].P(=O)(O)(O)O>CO>[CH3:1][N:2]([CH3:3])[C:7](=[O:13])[C:8]([O:10][CH3:11])=[O:9][CH3:1][NH:2][CH3:3].C[O-].[Na+].[C:7]([O:13]C)(=O)[C:8]([O:10][CH3:11])=[O:9].P(=O)(O)(O)O>CO>[CH3:1][N:2]([CH3:3])[C:7](=[O:13])[C:8]([O:10][CH3:11])=[O:9]In a 1,000 mL reactor are added at 0° C., 360 g (4 mol) of dimethylamine (DMA) solution at 50% by weight in methanol and 43.2 g (0.2 mol) of sodium methylate at 25% by weight in methanol. To this mixture are added at 0-5° C. and within 1 hour, 472 g (4 mol) of dimethyl oxalate. The mixture is maintained with stirring and at 0° C. for 2 hours. The reaction medium is concentrated in vacuo (Pmax=200 mbars) for removing residual DMA and methanol and an 85% orthophosphoric acid solution (23 g 0.2 mol) is then added. The salts formed are filtered and then the filtrate is distilled in vacuo (Tbp=68-70° C., P<1 mbar) in order to recover the desired product (461 g).
読み込み中…
