18-Sep-21 News New downstream synthetic route of 28485-17-8

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 28485-17-8, 5-Carbethoxyuracil.

Electric Literature of 28485-17-8, 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.

To a 100 ml three-necked flask was added ethyl uracil-5-carboxylate (2.2 g, 11.95 mmol)N, N-dimethylaniline (2 g, 16.50 mmol).Under ice bath, phosphorus oxychloride (9.2 g, 60 mmol) was gradually added and stirred continuously.After the addition of 10 minutes, gradually heating 110 C, and insulation 3h reaction.The reaction solution was slowly poured into an ice-water mixture (100 ml) and quenched and kept at a temperature below 5 C. And extracted twice with ethyl acetate (200 ml).The organic phases were combined, washed with saturated brine, dried and concentrated to give the crude product.The crude product was purified by column chromatography to give 1.8 g of solid in 68% yield.

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 28485-17-8, 5-Carbethoxyuracil.

Reference:
Patent; SUZHOU WANGSHAN WANGSHUI BIOMEDICAL CO LTD; TOPHARMAN SHANGHAI CO LTD; SHANDONG TOPHARMAN PHARMACEUTICAL CO LTD; TIAN, GUANGHUI; LI, JUNQI; (17 pag.)CN104650045; (2017); B;,
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Pyrimidine – Wikipedia

Brief introduction of 28485-17-8

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, 28485-17-8, 5-Carbethoxyuracil.

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 28485-17-8, name is 5-Carbethoxyuracil. This compound has unique chemical properties. The synthetic route is as follows. Application In Synthesis of 5-Carbethoxyuracil

A dry reaction flask equipped with a stirring bar and a reflux condenser was charged with 5-ethoxycarbonyluracil (1.84 g, 10 mmol), POCl3 (10 mL) and N,N-dimethylaniline (1 mL) and heated at 90 C. for 2 h. The excess POCl3 was removed under a reduced pressure and quenched with ice-water (100 g). The aqueous solution was extracted with ethyl ether (3×100 mL), washed with saturated aqueous NaHCO3 solution and water (100 mL, each). After drying over sodium sulfate, the ethyl ether was removed and the residue was dried under a high vacuum to afford 2,4-dichloro-5-ethoxycarbonylpyrimidine. 1H NMR (CDCl3): delta 9.00 (s, 1H), 4.45 (q, 2H, J=6.9 Hz), 1.42 (t, 3H, J=6.9 Hz).

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, 28485-17-8, 5-Carbethoxyuracil.

Reference:
Patent; RIGEL PHARMACEUTICALS, INC.; Singh, Rajinder; Argade, Ankush; Payan, Donald; Molineaux, Susan; Holland, Sacha; Clough, Jeffrey; Keim, Holger; Bhamidipati, Somasekhar; Sylvain, Catherine; Li, Hui; Rossi, Alexander; US2015/266828; (2015); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Brief introduction of 5-Carbethoxyuracil

According to the analysis of related databases, 28485-17-8, the application of this compound in the production field has become more and more popular.

Application of 28485-17-8, 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.

Step 2. A mixture of ethyl 2,4-dioxo-l,2,3,4-tetrahydropyrimidine-5-carboxylate obtained in step 1 (8.5 g, 46.2 mmol, 1.0 eq), N,N-dimethylbenzenamine (1.12 g, 9.24 mmol, 0.2 eq), POCl3 (21.25 g, 138.6 mmol, 3.0 eq) in benzene (300 mL) was stirred at 9O 0C under a nitrogen atmosphere for 8 h. The reaction mixture was allowed to cool to room temperature and throw into ice (300 g). The mixture was extracted by EtOAc (2×300 mL). The combined organic phases were washed (brine), dried (Na2SO4), filtered and concentrated. The residue was purified by silica gel chromatography (PE/EtOAc=500:l to 15:1 as eluent) to afford ethyl 2,4- dichloropyrimidine-5-carboxylate (3.83 g, 37%) as white solid. LC-MS (m/z) =220.9 [M+H]+.

According to the analysis of related databases, 28485-17-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; VERTEX PHARMACEUTICALS INCORPORATED; WANG, Tiansheng; HANZELKA, Brian; MUH, Ute; BEMIS, Guy; ZUCCOLA, Harmon, J.; WO2011/19405; (2011); A1;,
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Pyrimidine – Wikipedia

Analyzing the synthesis route of 5-Carbethoxyuracil

The synthetic route of 28485-17-8 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 28485-17-8, 5-Carbethoxyuracil, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, Formula: C7H8N2O4, blongs to pyrimidines compound. Formula: C7H8N2O4

Step i. Ethyl 2,4-dichloropyrimidine-5-carboxylate Under an N2 atmosphere, a mixture of 5-carbethoxyuracil (1.0 g, 5.4 mmol) and POCl3 (10 mL) was heated at reflux for 30 minutes. The solution was concentrated under reduced pressure to remove the excess of POCl3, and the residue was poured into ice (20 g). CH2Cl2 (100 mL) was added, and the mixture was basified to pH 9 using saturated aqueous NaHCO3 solution. The organic portion was dried over MgSO4 and concentrated to obtain ethyl 2,4-dichloropyrimidine-5-carboxylate as a yellow oil (900 mg, 75%).

The synthetic route of 28485-17-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Martinborough, Esther; Zimmermann, Nicole; Perni, Robert B.; Arnost, Michael; Bandarage, Upul K.; Maltais, Francois; Bemis, Guy; US2006/160817; (2006); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia

Analyzing the synthesis route of 28485-17-8

With the rapid development of chemical substances, we look forward to future research findings about 28485-17-8.

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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Pyrimidine – Wikipedia

Introduction of a new synthetic route about 28485-17-8

The synthetic route of 28485-17-8 has been constantly updated, and we look forward to future research findings.

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 28485-17-8, name is 5-Carbethoxyuracil, the common compound, a new synthetic route is introduced below. SDS of cas: 28485-17-8

Method for svnthesising A. Id; B.2a A.1*d A.1d; Caesium carbonate (1.77 g, 5.43 mmol) is suspended in 10 mL DMSO, combined with carboxylic acid ester B.l-lc (1.00 g, 5.43 mmol) and stirred for 10 min at 200C. Then methyl iodide (0.338 muL, 5.43 mmol) is added and the mixture is stirred for 16 h at 200C. The crude product is purified by RP chromatography and carboxylic acid ester B.l-ld (HPLC-MS: tRet. = 0.64 min; MS(M+H)+ = 199; method FEC3) is obtained.

The synthetic route of 28485-17-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; ENGELHARDT, Harald; BOEHMELT, Guido; KOFINK, Christiane; KUHN, Daniel; McCONNELL, Darryl; STADTMUELLER, Heinz; WO2010/7114; (2010); A2;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia