trimethyl ethane-1,1,2-tricarboxylate

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

実験手順: Trimethyl ethane-1,1,2-tricarboxylate (204 g, 1 mol) and acetamidine hydrochloride (95 g, mol) are added to a solution of sodium methylate (108 g, 2 mol) in methanol (600 ml) with stirring. The mixture is stirred for 16 hours at room temperature. Acidification with concentrated hydrochloric acid, filtration, washing with cold water and drying gives the methyl 4,6-dihydroxy-2-methyl-pyrimidin-5-yl-acetate (or tautomeric forms thereof) as a colorless solid (210 g), m.p.>200° C. The mixture is stirred for 16 hours at room temperature Acidification with concentrated hydrochloric acid, filtration washing with cold water drying

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

実験手順: Trimethyl ethane-1,1,2-tricarboxylate (204 g, 1 mol) and acetamidine hydrochloride (95 g, mol) are added to a solution of sodium methylate (108 g, 2 mol) in methanol (600 ml) with stirring. The mixture is stirred for 16 hours at room temperature. Acidification with concentrated hydrochloric acid, filtration, washing with cold water and drying gives the methyl 4,6-dihydroxy-2-methyl-pyrimidin-5-yl-acetate (or tautomeric forms thereof) as a colorless solid (210 g), m.p.>200° C. The mixture is stirred for 16 hours at room temperature Acidification with concentrated hydrochloric acid, filtration washing with cold water drying

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

実験手順: Trimethyl ethane-1,1,2-tricarboxylate (600 g, 3.0 mol) and formamidine acetate (312 g, 3.0 mol) are added sequentially to a vigourously stirred solution of sodium methylate (324 g, 6.0 mol) in methanol (1800 ml) at 0° C. The reaction mixture is stirred for 12 hours, diluted with t-butylmethyl ether (300 ml) and filtered with suction. The mixture of salts obtained is suspended in water (1000 ml) and acidified with concentrated hydrochloric acid (600 ml). Filtration and drying gives the methyl 4,6-dihydroxy-pyrimidin-5-yl-acetate or the tautomeric forms thereof as a white solid (420 g), m.p. >200° C. filtered with suction The mixture of salts obtained Filtration drying

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

実験手順: Trimethyl ethane-1,1,2-tricarboxylate (600 g, 3.0 mol) and formamidine acetate (312 g, 3.0 mol) are added sequentially to a vigourously stirred solution of sodium methylate (324 g, 6.0 mol) in methanol (1800 ml) at 0° C. The reaction mixture is stirred for 12 hours, diluted with t-butylmethyl ether (300 ml) and filtered with suction. The mixture of salts obtained is suspended in water (1000 ml) and acidified with concentrated hydrochloric acid (600 ml). Filtration and drying gives the methyl 4,6-dihydroxy-pyrimidin-5-yl-acetate or the tautomeric forms thereof as a white solid (420 g), m.p. >200° C. filtered with suction The mixture of salts obtained Filtration drying

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

実験手順: Trimethyl ethane-1,1,2-tricarboxylate (204 g, 1 mol) and acetamidine hydrochloride (95 g, 1 mol) are added to a solution of sodium methylate (108 g, 2 mol) in methanol (600 ml) with stirring. The mixture is stirred for 16 hours at room temperature. Acidification with concentrated hydrochloric acid, filtration, washing with cold water and drying gives the methyl 4,6-dihydroxy-2-methyl-pyrimidin-5-yl-acetate (or tautomeric forms thereof) as a colorless solid (210 g), m.p.>200° C. The mixture is stirred for 16 hours at room temperature Acidification with concentrated hydrochloric acid, filtration washing with cold water drying

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

実験手順: Trimethyl ethane-1,1,2-tricarboxylate (600 g, 3.0 mol) and formamidine acetate (312 g, 3.0 mol) are added sequentially to a vigourously stirred solution of sodium methylate (324 g, 6.0 mol) in methanol (1800 ml) at 0° C. The reaction mixture is stirred for 12 hours, diluted with t-butylmethyl ether (300 ml) and filtered with suction. The mixture of salts obtained is suspended in water (1000 ml) and acidified with concentrated hydrochloric acid (600 ml). Filtration and drying gives the methyl 4,6-dihydroxy-pyrimidin-5-yl-acetate or the tautomeric forms thereof as a white solid (420 g), m.p. >200° C. filtered with suction The mixture of salts obtained Filtration drying

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

実験手順: Trimethyl ethane-1,1,2-tricarboxylate (204 g, 1 mol) and acetamidine hydrochloride (95 g, mol) are added to a solution of sodium methylate (108 g, 2 mol) in methanol (600 ml) with stirring. The mixture is stirred for 16 hours at room temperature. Acidification with concentrated hydrochloric acid, filtration, washing with cold water and drying gives the methyl 4,6-dihydroxy-2-methyl-pyrimidin-5-yl-acetate (or tautomeric forms thereof) as a colorless solid (210 g), m.p.>200° C. The mixture is stirred for 16 hours at room temperature Acidification with concentrated hydrochloric acid, filtration washing with cold water drying

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

実験手順: Trimethyl ethane-1,1,2-tricarboxylate (600 g, 3.0 mol) and formamidine acetate (312 g, 3.0 mol) are added sequentially to a vigourously stirred solution of sodium methylate (324 g, 6.0 mol) in methanol (1800 ml) at 0° C. The reaction mixture is stirred for 12 hours, diluted with t-butylmethyl ether (300 ml) and filtered with suction. The mixture of salts obtained is suspended in water (1000 ml) and acidified with concentrated hydrochloric acid (600 ml). Filtration and drying gives the methyl 4,6-dihydroxy-pyrimidin-5-yl-acetate or the tautomeric forms thereof as a white solid (420 g), m.p. >200° C. filtered with suction The mixture of salts obtained Filtration drying