5-acetyl-1,3-dimethyl-1,3-diazinane-2,4,6-trione

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 1.5 g of 5-acetyl-1,3-dimethylbarbituric acid was dissolved in 50 ml of ethanol and 1.5 ml of ethoxyamine was added to it. After the resulting solution was stirred at 40° C during 2 hours, it was allowed to stand at a room temperature. The separated white plates were filtered and recrystallized from ethanol, and thereby 1.4 g of the desired compound was obtained. to stand at a room temperature The separated white plates were filtered recrystallized from ethanol

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 1,3-dimethylbarbituric acid (10 g, 64.04 mmol), 4-dimethylaminopyridine (9.49 g, 158.0 mmol) in dry CH2Cl2 (190 ml) was cooled to 0° C. and acetic anhydride (7.35 ml, 77.9 mmol) added dropwise in 15 min. The reaction mixture was stirred overnight at room temperature, diluted with CH2Cl2 (500 ml) and washed with 2 N HCl solution (80 ml). The organic phase was dried over MgSO4 and evaporated. The residue was crystallised from MeOH, giving 5-acetyl-1,3-dimethyl-2,4,6(1H,3H,5H)-pyrimidinetrione 1 (8.6 g, 68%). washed with 2 N HCl solution (80 ml) The organic phase was dried over MgSO4 evaporated The residue was crystallised from MeOH