Method for synthesizing 4,6-dichloro-2-(propylthio)-5-aminopyrimidine
A technology of aminopyrimidine and propylthio, which is applied in the field of synthesizing 4,6-dichloro-2--5-aminopyrimidine, which can solve the problems of cumbersome operation, harsh reaction conditions, and high price, and achieve short route and simple operation , low-cost effect
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Embodiment 12
[0042] Example 12 Synthesis of 4,6-trihydroxy-5-acetamidopyrimidine (IVa)
[0043] Mix 50.0 g of diethyl acetamidomalonate (III), 28.8 g of urea, 77.0 g of sodium ethoxide and 750 mL of ethanol at room temperature, and react under reflux for 15 hours. After the reaction, filter, wash the filter cake with 50 mL ethanol, and collect the filter cake. Dissolve the obtained solid with 1L of water and adjust the pH to neutral with hydrochloric acid. A solid precipitated out. After the solid was separated and fully dried, 39.3g of 2,4,6-trihydroxy-5-acetamidopyrimidine (IVa) was obtained. Next reaction. ESI-MSm / z:186[M+H] + ; 1 HNMR(400MHz, D 2 O) δ 2.13 (s, 3H).
Embodiment 22
[0044] Example 22 Synthesis of 4,6-trihydroxy-5-benzamidopyrimidine (IVb)
[0045] At room temperature, 6.43 g of diethyl benzamidomalonate (III), 2.9 g of urea, 7.7 g of sodium ethoxide and 75 mL of ethanol were mixed with each other, and reacted under reflux for 13 hours. After the reaction, the solvent was removed under reduced pressure, and 100 mL of water was added. The pH was adjusted to neutral with hydrochloric acid, and the aqueous solution was extracted with 200 mL of chloroform, repeated 3 times, and the chloroform layers were combined. After drying, the solvent was removed to obtain 5 g of an oily substance containing 2,4,6-trihydroxy-5-benzamidopyrimidine (IVb), which was directly subjected to the next reaction. ESI-MSm / z:248[M+H] + .
Embodiment 32
[0046] Example 32 Synthesis of,4,6-Trichloro-5-aminopyrimidine (Ⅴ)
[0047] 33.0 g of the crude compound (IVa) obtained in Example 1, 21.2 g of pyridine and 500 mL of toluene were mixed with each other, and then 62.2 g of phosphorus oxychloride was added, and the mixture was heated and refluxed for 24 hours. After the reaction is complete, concentrate to remove the solvent and most of the remaining phosphorus oxychloride. The residue was poured into ice water, and extracted twice with 500 mL ethyl acetate. After the organic phases were combined, they were washed once with 300 mL of saturated sodium bicarbonate solution. The organic phase was dried and concentrated to obtain 35.1 g of an oily substance containing 2,4,6-trichloro-5-aminopyrimidine (V). ESI-MSm / z:199[M+H] + .
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