As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 28485-17-8, name is 5-Carbethoxyuracil, molecular formula is C7H8N2O4, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. HPLC of Formula: C7H8N2O4
EXAMPLE 5 In 200 ml. of water is suspended 920 mg. of ethyl 1,2,3,4-tetrahydro-2,4-dioxopyrimidine-5-carboxylate and, while the suspension is stirred vigorously at room temperature, a gaseous mixture of fluorine (25 V/V%) and nitrogen is introduced. In the course, the starting material dissolves to yield a homogeneous solution. When 2.6 mole equivalents of said gaseous mixture has been introduced, the ultraviolet absorption spectrum of the reaction mixture is measured. When the absence of unreacted starting compounds is confirmed by the spectrum, the reaction is stopped. Following addition of 1.10 g. of calcium carbonate, the reaction mixture is stirred for a while, after which the insolubles are filtered off. The filtrate is concentrated to dryness under reduced pressure, whereupon a white solid is obtained. This product is suspended in 50 ml. of acetone and the insolubles are filtered off. The acetone-solubles are subjected to column chromatography on silica gel (solvent: chloroform containing 1.5 V/V% of methanol), followed by concentration of the fraction containing the desired compound under reduced pressure to recover a white solid product. Recrystallization from methanol-chloroformhexane yields 561 mg. of colorless prisms of ethyl 5-fluoro-6-hydroxy-1,2,3,4,5,6-hexahydro-2,4-dioxopyrimidine-5-carboxylate. melting point: 163-165 C. NMR spectrum (DMSO-d6) delta: 1.22(3H,t, J=7HZ), 4.28(2H, q, J=7HZ), 4.93(1H, d*d, JHF =3HZ, J=5HZ; after addition of deuterium oxide, d, JHF =3HZ), 6.3(1H, broad), 8.48(1H, broad), 10.80(1H, broad). Elemental analysis, for C7 H9 FN2 O5: Calcd.: C, 38.19; H, 4.12; N, 12.73. Found: C, 37.90; H, 3.94; N, 12.87.
With the rapid development of chemical substances, we look forward to future research findings about 28485-17-8.
Reference:
Patent; Takeda Chemical Industries, Ltd.; US4329460; (1982); A;,
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