5,6-Diamino-1-methyluracil

Yellow solid

To further increase the conversion rate of the reaction, Catalytic reduction of 6-amino-5-nitroso-1-methyluracil The reaction system of 5, 6-diamino-1-methyluracil was optimized, and in order to obtain a high separation yield, the post-reaction treatment was also optimized. The optimized steps were: 1) 0.4 g of ammonium metatungstate modified palladium metal catalyst (prepared in Example 1), Substrate 6-amino-5-nitroso-1-methyl uracil 10.0g was added to 80ml of isopropanol and stirred in the hydrogenation reactor; 2) Nitrogen replaces the air in the hydrogenation reactor three times, and then adjusts the temperature of the hydrogenation reactor to 55°C. (Hydrogen pressure is 0.3 MPa), the reaction was taken 2h after the reaction solution was subjected to HPLC (HPLC assay result was 99.6percent conversion, selectivity 98.3percent), stirring was stopped, hydrogen pressure was removed, and the temperature was lowered to room temperature; 3) Filtrate, remove the catalyst by filtration, collect the filtrate and heat up to 50-60 °C (after treatment; 4) Add purified water to the post-treatment solution, stop the dripping when turbidity has appeared, and incubate for 2h, then continue dropping. When water is no longer crystallized (a total of 45 ml of water is dropped, 10 ml is added when turbid, and 35 ml is added dropwise), the temperature is lowered to 10° C., filtered and dried to give pale yellow 5, 6-diamino-1 -methyl uracil ( The weight yield was 92.3percent, and the volume purity was 99.4percent).6-Amino-5-nitroso-1-methyluracil 2a (11.50 g, 67.6 mmol) was dissolved in 200 mL of aqueous ammonia (25percent)in, Sodium dithionite (41.20 g, 236.6 mmol) was added at room temperature 25 ° C and stirred. The temperature in the reaction flask was gradually increased to 35 °C. When the temperature inside the bottle no longer rises, it is heated to 60 ° C and stirred for 1 h.The reaction was then moved to room temperature and stirred for 6 h. After the reaction was completed, the stirring was stopped, filtered, and the cake was washed with ice water and dried in vacuo. Intermediate 3a was obtained as a white solid 9.28 g, yield 87.9percent.6-Amino-1-methylpyrimidine-2, 4-dione (10.0 g, 70.1 mmol) was dissolved in water (100 mL). 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.

Theobromine intermediates.

Molecular Weight:156.14
XLogP3:-1.4
Hydrogen Bond Donor Count:3
Hydrogen Bond Acceptor Count:4
Exact Mass:156.06472551
Monoisotopic Mass:156.06472551
Topological Polar Surface Area:101
Heavy Atom Count:11
Complexity:257
Covalently-Bonded Unit Count:1
Compound Is Canonicalized:Yes