| 93% |
With hydrogenchloride; sodium nitrite; In water; at 0 - 25℃; for 2h; |
6-Amino-1-methylpyrimidine-2,4-dione (10.0 g, 70.1 mmol) was dissolved in water (100 mL). Hydrochloric acid (7 mL, 84.0 mmol, 12 N) was added dropwise at 0C while stirring. Then sodium nitrite (5.80 g, 84.2 mmol) was dissolved in water (50 mL) and added dropwise to the reaction solution to give a purple precipitate. The reaction was stirred at 25C for 2 hours, filtered and washed with cold water to give a purple solid. The solid was dissolved in water (100 mL) and sodium hydrosulphite (18.7 g, 118 mmol) was added in batches while stirring, heated to 60C and stirred for 0.5 h, cooled to 25C and stirred for 16 h, filtered, washed with cold water (50 mL), ethanol (50 mL), acetone (50 mL) respectively, and dried to give 5,6-diamino-1-methylpyrimidine-2,4-dione (8.60 g, as a pale yellow solid) with a yield of 93%. 1H NMR (400 MHz, DMSO-d6) delta 10.49(br, 1H), 6.15(br, 2H), 3.25(s, 3H), 2.95(br, 2H). MS-ESI calcd. [M + H]+ 157, found 157. |
| 93% |
With hydrogenchloride; sodium nitrite; In water; at 0 - 25℃; for 2h; |
6-Amino-1-methylpyrimidin-2,4-dione (10.0 g, 70.1 mmol) was dissolved in water (100 mL), and then hydrochloric acid (7 mL, 84.0 mmol, 12N) was added dropwise at 0 C. while stirring. Sodium nitrite (5.80 g, 84.2 mmol) was dissolved in water (50 mL), which was added dropwise into the reactants, then a purple precipitate appeared. The reaction solution was stirred 25 C. for 2 hours, the then was filtered. The filtrate was washed with cold water to give a purple solid. The solid was dissolved in water (100 mL), and then sodium hypodisulfite (18.7 g, 118 mmol) was added in batches while stirring. The reaction solution was heated to 60 C. and stirred for 0.5 hour, and then was cooled to 25 C. and stirred for 16 hours. The reaction solution was filtered and the filtrate was washed with water (50 mL), ethanol (50 mL) and propanone (50 mL), respectively, followed by drying to give a product 5,6-diamino-1-methylpyrimidin-2,4-dione (8.60 g, pale yellow solid), with a yield of 93%. 1H NMR (400 MHz, DMSO-d6) delta10.49 (s, 1H), 6.15 (s, 2H), 3.25 (s, 3H), 2.95 (s, 2H). MS-ESI calculated value: [M+H]+ 157; measured value: 157. |
| 78% |
With ammonium hydroxide; sodium dithionite; at 50℃; for 1h; |
The purple solid (3 g, 17.6 mmol) and 25% aqueous ammonia (30 ml) were added to a 100 ml reaction flask, and sodium dithionite (10.8 g, 61.6 mmol) was added in portions and stirred at 50 C for 1 h, and the reaction solution was cooled to room temperature. The reaction was stirred at room temperature for 8 h, filtered, and the filter cake was washed with ice water (10 ml) and icedLight yellow solid (2.15g, 78%) |
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